2-pyrrolidin-1-ylethylhydrazine

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

実験手順: A mixture of 200 g of 85% hydrazine hydrate, 200 ml of water, 170 g of N-chloroethylpyrrolidine hydrochloride, and 70 g of potassium carbonate was boiled under reflux for seven hours. Sodium hydroxide (390 g) was added and the mixture was extracted with ether. The ethereal extract, dried and distilled, yielded the title compound, bp 107°-111° C. (18.5 mm). under reflux for seven hours the mixture was extracted with ether The ethereal extract dried distilled

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

実験手順: A mixture of 12.2 g of 1-chloro-7-methoxy-4-nitro-9H-xanthen-9-one and 11.0 g of 1-(2-hydrazinoethyl)pyrrolidine in 200 ml of THF was stirred 20 hours at room temperature. The orange liquor was decanted, freed of solvent under reduced pressure, and the residue, in chloroform, was chromatographed over silica gel, eluting with chloroform-methanol (25:1 by volume). The desired fractions yielded the free base of the title compound, mp 140°-142° C. The orange liquor was decanted the residue, in chloroform, was chromatographed over silica gel eluting with chloroform-methanol (25:1 by volume)

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

実験手順: A mixture of 200 g of 85% hydrazine hydrate, 200 ml of water, 170 g of N-chloroethylpyrrolidine hydrochloride, and 70 g of potassium carbonate was boiled under reflux for seven hours. Sodium hydroxide (390 g) was added and the mixture was extracted with ether. The ethereal extract, dried and distilled, yielded the title compound, bp 107°-111° C. (18.5 mm). under reflux for seven hours the mixture was extracted with ether The ethereal extract dried distilled

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

実験手順: A mixture of 200 g of 85% hydrazine hydrate, 200 ml of water, 170 g of N-chloroethylpyrrolidine hydrochloride, and 70 g of potassium carbonate was boiled under reflux for seven hours. Sodium hydroxide (390 g) was added and the mixture was extracted with ether. The ethereal extract, dried and distilled, yielded the title compound, bp 107°-111° C. (18.5 mm). under reflux for seven hours the mixture was extracted with ether The ethereal extract dried distilled

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

実験手順: A mixture of 12.2 g of 1-chloro-7-methoxy-4-nitro-9H-xanthen-9-one and 11.0 g of 1-(2-hydrazinoethyl)pyrrolidine in 200 ml of THF was stirred 20 hours at room temperature. The orange liquor was decanted, freed of solvent under reduced pressure, and the residue, in chloroform, was chromatographed over silica gel, eluting with chloroform-methanol (25:1 by volume). The desired fractions yielded the free base of the title compound, mp 140°-142° C. The orange liquor was decanted the residue, in chloroform, was chromatographed over silica gel eluting with chloroform-methanol (25:1 by volume)

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

実験手順: A mixture of 12.2 g of 1-chloro-7-methoxy-4-nitro-9H-xanthen-9-one and 11.0 g of 1-(2-hydrazinoethyl)pyrrolidine in 200 ml of THF was stirred 20 hours at room temperature. The orange liquor was decanted, freed of solvent under reduced pressure, and the residue, in chloroform, was chromatographed over silica gel, eluting with chloroform-methanol (25:1 by volume). The desired fractions yielded the free base of the title compound, mp 140°-142° C. The orange liquor was decanted the residue, in chloroform, was chromatographed over silica gel eluting with chloroform-methanol (25:1 by volume)

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

実験手順: A mixture of 200 g of 85% hydrazine hydrate, 200 ml of water, 170 g of N-chloroethylpyrrolidine hydrochloride, and 70 g of potassium carbonate was boiled under reflux for seven hours. Sodium hydroxide (390 g) was added and the mixture was extracted with ether. The ethereal extract, dried and distilled, yielded the title compound, bp 107°-111° C. (18.5 mm). under reflux for seven hours the mixture was extracted with ether The ethereal extract dried distilled

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

実験手順: A mixture of 12.2 g of 1-chloro-7-methoxy-4-nitro-9H-xanthen-9-one and 11.0 g of 1-(2-hydrazinoethyl)pyrrolidine in 200 ml of THF was stirred 20 hours at room temperature. The orange liquor was decanted, freed of solvent under reduced pressure, and the residue, in chloroform, was chromatographed over silica gel, eluting with chloroform-methanol (25:1 by volume). The desired fractions yielded the free base of the title compound, mp 140°-142° C. The orange liquor was decanted the residue, in chloroform, was chromatographed over silica gel eluting with chloroform-methanol (25:1 by volume)