butyl 2-aminoacetate;hydrochloride

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated

反応条件: temp:250.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solid mixture of 4-(pyridin-4-ylsulfanyl)-phthalic acid (11.40 g) and glycine n-butyl ester hydrochloride salt (6.95 g) was heated in a oil bath (250° C.) with efficient stirring for 20 min. until the water bubble evaporation ceased. After cooling, it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml). Two layers were separated and the aqueous layer was extracted with ethyl acetate (300 ml). Combined organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound 10.70 g. MS-(+)-ion: M+1=371.2. bubble evaporation After cooling it was partitioned between ethyl acetate (300 ml) and saturated sodium bicarbonate aqueous solution (150 ml) Two layers were separated the aqueous layer was extracted with ethyl acetate (300 ml) Combined organic layers were washed with brine dried over magnesium sulfate filtered concentrated