2-(trichloromethyl)oxirane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A stirred mixture of 5-bromopyrimid-2-one (0.009 mol), 1,2-epoxy-3,3,3-trichloropropane (0.009 mol) and K2CO3 (33 mg) in dimethylformamide (40 ml ) was heated at 80° C. for 4 h. The reaction mixture was then evaporated to dryness at reduced pressure (1 mm Hg). The crystalline residue was triturated with a little ether and dissolved in ethyl acetate. The filtered ethyl acetate solution was concentrated to about 50 ml and left in the cold when the product crystallized out in 52% yield. m.p. 210°-212° C. (ethyl acetate). The reaction mixture was then evaporated to dryness at reduced pressure (1 mm Hg) The crystalline residue was triturated with a little ether dissolved in ethyl acetate The filtered ethyl acetate solution was concentrated to about 50 ml left in the cold when the product crystallized out in 52% yield

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

実験手順: To 200 grams of stirred methanol were added 48.4 grams of 2-(trichloromethyl)oxirane and 21.9 grams of 1,1-dimethylethylamine at equimolar rates, dropwise, at 20° C. during 30 minutes. After stirring 16 hours at ambient temperature, the solvent was removed under reduced pressure of 100 mm. Hg and the white residue recrystallized from 300 grams of hexane to yield 50.7 grams of 3-(1,1-dimethylethylamino)-1,1,1-trichloro-2-propanol melting 100.5°-102° C. the solvent was removed under reduced pressure of 100 mm. Hg the white residue recrystallized from 300 grams of hexane

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

実験手順: The preparation of 2-(trichloromethyl)oxirane is reported by H. Gilman and R. K. Abbott, Jr., J. Org. Chem. 8, 224 (1943). 2-(Trichloromethyl)oxirane can be reacted with 1,1-dimethylethylamine at about -30° to +50° C. in a solvent such as methanol to produce 3-(1,1-dimethylethylamino)-1,1,1-trichloro-2-propanol.

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: To 200 grams of stirred methanol were added 48.4 grams of 2-(trichloromethyl)oxirane and 21.9 grams of 1,1-dimethylethylamine at equimolar rates, dropwise, at 20° C. during 30 minutes. After stirring 16 hours at ambient temperature, the solvent was removed under reduced pressure of 100 mm. Hg and the white residue recrystallized from 300 grams of hexane to yield 50.7 grams of 3-(1,1-dimethylethylamino)-1,1,1-trichloro-2-propanol melting 100.5°-102° C. the solvent was removed under reduced pressure of 100 mm. Hg the white residue recrystallized from 300 grams of hexane

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

実験手順: The preparation of 2-(trichloromethyl)oxirane is reported by H. Gilman and R. K. Abbott, Jr., J. Org. Chem. 8, 224 (1943). 2-(Trichloromethyl)oxirane can be reacted with 1,1-dimethylethylamine at about -30° to +50° C. in a solvent such as methanol to produce 3-(1,1-dimethylethylamino)-1,1,1-trichloro-2-propanol.

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

実験手順: N-methyl piperazine (2 g) is dissolved in 80 ml chloroform, and mixed with a solution of 3.22 g 3,3,3-trichloropropylene oxide in 20 ml chloroform. The mixture is allowed to stand at room temperature for 6 days. The chloroform is removed by evaporation, and ether is added to the residue, which is then collected by filtration, washed with ether and dried at room temperature under water pump vacuum, to give the heading compound, m.p. 165°-167° C. The chloroform is removed by evaporation, and ether is added to the residue, which is then collected by filtration washed with ether dried at room temperature under water pump vacuum to give the heading compound, m.p. 165°-167° C.

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A stirred mixture of 5-bromopyrimid-2-one (0.009 mol), 1,2-epoxy-3,3,3-trichloropropane (0.009 mol) and K2CO3 (33 mg) in dimethylformamide (40 ml ) was heated at 80° C. for 4 h. The reaction mixture was then evaporated to dryness at reduced pressure (1 mm Hg). The crystalline residue was triturated with a little ether and dissolved in ethyl acetate. The filtered ethyl acetate solution was concentrated to about 50 ml and left in the cold when the product crystallized out in 52% yield. m.p. 210°-212° C. (ethyl acetate). The reaction mixture was then evaporated to dryness at reduced pressure (1 mm Hg) The crystalline residue was triturated with a little ether dissolved in ethyl acetate The filtered ethyl acetate solution was concentrated to about 50 ml left in the cold when the product crystallized out in 52% yield

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

実験手順: To 200 grams of stirred methanol were added 48.4 grams of 2-(trichloromethyl)oxirane and 21.9 grams of 1,1-dimethylethylamine at equimolar rates, dropwise, at 20° C. during 30 minutes. After stirring 16 hours at ambient temperature, the solvent was removed under reduced pressure of 100 mm. Hg and the white residue recrystallized from 300 grams of hexane to yield 50.7 grams of 3-(1,1-dimethylethylamino)-1,1,1-trichloro-2-propanol melting 100.5°-102° C. the solvent was removed under reduced pressure of 100 mm. Hg the white residue recrystallized from 300 grams of hexane

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

実験手順: The preparation of 2-(trichloromethyl)oxirane is reported by H. Gilman and R. K. Abbott, Jr., J. Org. Chem. 8, 224 (1943). 2-(Trichloromethyl)oxirane can be reacted with 1,1-dimethylethylamine at about -30° to +50° C. in a solvent such as methanol to produce 3-(1,1-dimethylethylamino)-1,1,1-trichloro-2-propanol.