N-ethylacetamide

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Ethyl-acetamide (1.18 g, 0.0135 m) in dry dimethylformamide (10 ml) was stirred at room temperature under nitrogen during the portionwise addition of 50% sodium hydride/oil dispersion (0.65 g, 0.0135 m). After the addition, the mixture was warmed to 50° C. and then 4-methyl-2-phenylmethylsulphinyloxazole (3.0 g, 0.0135 m) was added. The mixture was stirred at 50° C. for 5 hours and then hydrolysed with water. The solvent was evaporated in vacuo and the residue extracted with diethyl ether. Column chromatography on silica using ether gave a pale yellow oil which gave the title product as a colourless oil on distillation, b.p. 50°-51° C./0.05 mm. After the addition The solvent was evaporated in vacuo the residue extracted with diethyl ether gave a pale yellow oil which

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Ethyl-acetamide (1.18 g, 0.0135 m) in dry dimethylformamide (10 ml) was stirred at room temperature under nitrogen during the portionwise addition of 50% sodium hydride/oil dispersion (0.65 g, 0.0135 m). After the addition, the mixture was warmed to 50° C. and then 4-methyl-2-phenylmethylsulphinyloxazole (3.0 g, 0.0135 m) was added. The mixture was stirred at 50° C. for 5 hours and then hydrolysed with water. The solvent was evaporated in vacuo and the residue extracted with diethyl ether. Column chromatography on silica using ether gave a pale yellow oil which gave the title product as a colourless oil on distillation, b.p. 50°-51° C./0.05 mm. After the addition The solvent was evaporated in vacuo the residue extracted with diethyl ether gave a pale yellow oil which

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

実験手順: N-Ethyl-acetamide (10.0 g, 0.115 m) in dry butyl hexyl ether (50 ml) was stirred at room temperature under nitrogen during the dropwise addition of a 1.445 M solution of n-butyl lithium in hexane (79.6 ml, 0.115 m). After the addition, the mixture was stirred for 15 minutes and then a solution of 4,5-dimethyl-2-methylsulphonyloxazole (20.0 g, 0.114 m) in dry butyl hexyl ether (50 ml) was added dropwise. The mixture was stirred for 2 hours at room temperature. Isolation of the product and distillation gave a colourless oil, b.p. 61°-62° C/0.3 mm. After the addition The mixture was stirred for 2 hours at room temperature Isolation of the product and distillation gave a colourless oil, b.p. 61°-62° C/0.3 mm

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

実験手順: Into a mixture of 87 gm of N-ethylacetamide and 82 gm of phosphorous acid, hydrogen chloride was introduced for 8 hours. During this time the mixture was stirred and the temperature was held at 150° - 160° C. The reaction mixture was then treated analogously to Example 1, and the N-ethyl-1-aminoethane- 1,1 -diphosphonic acid product was obtained. The yield was 36.5 gm. was introduced for 8 hours was held at 150° - 160° C The reaction mixture was then treated analogously to Example 1

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

実験手順: Into a mixture of 87 gm of N-ethylacetamide and 82 gm of phosphorous acid, hydrogen chloride was introduced for 8 hours. During this time the mixture was stirred and the temperature was held at 150° - 160° C. The reaction mixture was then treated analogously to Example 1, and the N-ethyl-1-aminoethane- 1,1 -diphosphonic acid product was obtained. The yield was 36.5 gm. was introduced for 8 hours was held at 150° - 160° C The reaction mixture was then treated analogously to Example 1

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

実験手順: The title compound was prepared from 1-[4-(chloromethyl)phenyl]-3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazole and N-ethylacetamide using a similar procedure to that described for Description 15.

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

実験手順: The title compound was prepared from 1-[4-(chloromethyl)phenyl]-3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazole and N-ethylacetamide using a similar procedure to that described for Description 15.

反応条件: temp:0.00; pressure:0.00; stir: