1,3-diazinane-2-thione

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: A solution of 2.9 grams of 1-bromo-1,3-diphenyl-2-propanone (Example 93) in 30 ml. of acetone is added to a solution of 1.16 grams of tetrahydro-2-pyrimidinethione in 100 ml. of acetone. A white precipitate forms in a few minutes. After standing at room temperature for four hours, the precipitate is collected, washed with acetone, and dried. Recrystallization from 20 ml. of ethanol yields 2.3 grams of the pure compound, melting at 192°-194° C. with decomposition. A white precipitate forms in a few minutes the precipitate is collected washed with acetone dried Recrystallization from 20 ml

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

実験手順: A 2.1 g. portion of 1,1-diphenyl-2-propanone is converted to 1-bromo-3,3-diphenyl-2-propanone by the procedure of Example 22. The 1-bromo-3,3-diphenyl-2-propanone is dissolved in 15 ml. of acetone and added to a boiling mixture of 0.80 g. of tetrahydro-2-pyrimidinethione in 70 ml. of acetone. This mixture is allowed to stand for 48 hours and the resulting solid is collected by filtration, giving the desired product, m.p. 196°-198° C. the resulting solid is collected by filtration

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

実験手順: The reaction mixture comprising one equivalent of 3,4,5,6-tetrahydro(1H)pyrimidine-2-thione and 1.2 equivalents of iodomethane in methanol (10 ml/g of thio-urea) is heated under reflux for 5 hours. After cooling down, the methanol is evaporated off under reduced pressure in order to quantitatively produce the product. The precipitate can then be washed in acetone or petroleum ether. under reflux for 5 hours After cooling down the methanol is evaporated off under reduced pressure in order to quantitatively produce the product The precipitate can then be washed in acetone

反応条件: temp:4.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The preparation of the starting material, 1,4,5,6-tetrahydropyrimidin-2-ylhydrazine hydrochloride, is carried out as follows: 1,4,5,6-tetrahydropyrimidin-2-thione and methyl chloride (excess) are added to isopropanol and the mixture heated in an autoclave at 170°-180° C. for hours. Cooling to 4° C. yields a precipitate of 2-methylthio-1,4,5,6-tetrahydropyrimidine hydrochloride, which upon treatment with hydrazine in boiling ethanol yields the desired intermediate melting at 191°-192° C. the mixture heated in an autoclave at 170°-180° C. for hours

反応条件: temp:4.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The preparation of the starting material, 1,4,5,6-tetrahydropyrimidin-2-ylhydrazine hydrochloride, is carried out as follows: 1,4,5,6-tetrahydropyrimidin-2-thione and methyl chloride (excess) are added to isopropanol and the mixture heated in an autoclave at 170°-180° C. for hours. Cooling to 4° C. yields a precipitate of 2-methylthio-1,4,5,6-tetrahydropyrimidine hydrochloride, which upon treatment with hydrazine in boiling ethanol yields the desired intermediate melting at 191°-192° C. the mixture heated in an autoclave at 170°-180° C. for hours

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: A solution of 2.9 grams of 1-bromo-1,3-diphenyl-2-propanone (Example 93) in 30 ml. of acetone is added to a solution of 1.16 grams of tetrahydro-2-pyrimidinethione in 100 ml. of acetone. A white precipitate forms in a few minutes. After standing at room temperature for four hours, the precipitate is collected, washed with acetone, and dried. Recrystallization from 20 ml. of ethanol yields 2.3 grams of the pure compound, melting at 192°-194° C. with decomposition. A white precipitate forms in a few minutes the precipitate is collected washed with acetone dried Recrystallization from 20 ml

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

実験手順: A 2.1 g. portion of 1,1-diphenyl-2-propanone is converted to 1-bromo-3,3-diphenyl-2-propanone by the procedure of Example 22. The 1-bromo-3,3-diphenyl-2-propanone is dissolved in 15 ml. of acetone and added to a boiling mixture of 0.80 g. of tetrahydro-2-pyrimidinethione in 70 ml. of acetone. This mixture is allowed to stand for 48 hours and the resulting solid is collected by filtration, giving the desired product, m.p. 196°-198° C. the resulting solid is collected by filtration

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

実験手順: A solution of 2.9 grams of 1-bromo-1,3-diphenyl-2-propanone (Example 93) in 30 ml. of acetone is added to a solution of 1.16 grams of tetrahydro-2-pyrimidinethione in 100 ml. of acetone. A white precipitate forms in a few minutes. After standing at room temperature for four hours, the precipitate is collected, washed with acetone, and dried. Recrystallization from 20 ml. of ethanol yields 2.3 grams of the pure compound, melting at 192°-194° C. with decomposition. A white precipitate forms in a few minutes the precipitate is collected washed with acetone dried Recrystallization from 20 ml

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

実験手順: A 2.1 g. portion of 1,1-diphenyl-2-propanone is converted to 1-bromo-3,3-diphenyl-2-propanone by the procedure of Example 22. The 1-bromo-3,3-diphenyl-2-propanone is dissolved in 15 ml. of acetone and added to a boiling mixture of 0.80 g. of tetrahydro-2-pyrimidinethione in 70 ml. of acetone. This mixture is allowed to stand for 48 hours and the resulting solid is collected by filtration, giving the desired product, m.p. 196°-198° C. the resulting solid is collected by filtration

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

実験手順: The reaction mixture comprising one equivalent of 3,4,5,6-tetrahydro(1H)pyrimidine-2-thione and 1.2 equivalents of iodomethane in methanol (10 ml/g of thio-urea) is heated under reflux for 5 hours. After cooling down, the methanol is evaporated off under reduced pressure in order to quantitatively produce the product. The precipitate can then be washed in acetone or petroleum ether. under reflux for 5 hours After cooling down the methanol is evaporated off under reduced pressure in order to quantitatively produce the product The precipitate can then be washed in acetone