5-甲基-1,4,5,6-四氢-1,3,5-三嗪-2-硫醇

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-bromo-3-(m-nitrobenzoyl)propionic acid (7.55 g, 0.024 mole) in methanol (50 ml) was mixed with a solution of 5-methyl-3,4,5,6-tetrahydro-s-triazine-2(1H)thione (3.27 g, 0.025 mole) in the same solvent (170 ml). After 3 hours at room temperature the solvent was evaporated to small volume when a colourless solid crystallised, which was collected to give 7-carboxymethyl-6-hydroxy-3-methyl-6-(m-nitrophenyl)-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide methanolate (7.5 g), m.p. 144°-145° C. (decomposition). After 3 hours at room temperature the solvent was evaporated to small volume when a colourless solid crystallised which was collected

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-bromo-3-(m-nitrobenzoyl)propionic acid (7.55 g, 0.024 mole) in methanol (50 ml) was mixed with a solution of 5-methyl-3,4,5,6-tetrahydro-s-triazine-2(1H)thione (3.27 g, 0.025 mole) in the same solvent (170 ml). After 3 hours at room temperature the solvent was evaporated to small volume when a colourless solid crystallised, which was collected to give 7-carboxymethyl-6-hydroxy-3-methyl-6-(m-nitrophenyl)-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide methanolate (7.5 g), m.p. 144°-145° C. (decomposition). After 3 hours at room temperature the solvent was evaporated to small volume when a colourless solid crystallised which was collected

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-bromo-3-(p-chlorobenzoyl) propionic acid (7.29 g, 0.025 moles) in methanol (40 ml) was mixed with a solution of 5-methyl-3,4,5,6-tetrahydro-s-triazin-2(1H)-thione (3.27 g, 0.025 moles) in the same solvent (150 ml) and left for one hour. Evaporation of the solvent gave 7-carboxymethyl-6-(p-chlorophenyl)-6-hydroxy-3-methyl-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide as a pale yellow solid (9.6 g), m.p. 111°-113° C. Evaporation of the solvent

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-bromo-3-(p-chlorobenzoyl) propionic acid (7.29 g, 0.025 moles) in methanol (40 ml) was mixed with a solution of 5-methyl-3,4,5,6-tetrahydro-s-triazin-2(1H)-thione (3.27 g, 0.025 moles) in the same solvent (150 ml) and left for one hour. Evaporation of the solvent gave 7-carboxymethyl-6-(p-chlorophenyl)-6-hydroxy-3-methyl-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide as a pale yellow solid (9.6 g), m.p. 111°-113° C. Evaporation of the solvent

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-benzoyl-3-bromo-propionic acid (6.4 g, 0.025 moles) in methanol (30 ml) was mixed with a solution of 5-methyl-3,4,5,6-tetrahydro-s-triazine-2(1H)-thione (3.27 g, 0.025 moles) in the same solvent (100 ml) and left for 3 hours. Evaporation of the solvent gave 7-carboxymethyl-6-hydroxy-3-methyl-6-phenyl-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide quarter hydrate as a pale yellow solid (8.8 g), m.p. 74°-77° C. Evaporation of the solvent

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 6.95 grams (0.025 moles) of p-bromophenacylbromide in 60 milliliters of acetone was mixed with a solution of 3.27 grams (0.025 moles) of 3,4,5,6-tetrahydro-5-methyl-s-triazin 2(1H) thione in 450 milliliters of acetone. 6-p-Bromophenyl-6-hydroxy-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a-]-s-triazine hydrobromide crystallized out as a colourless solid, m.p. 138°-140° C. (decomposition). The yield was 7.5 grams (75%). 6-p-Bromophenyl-6-hydroxy-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a-]-s-triazine hydrobromide crystallized out as a colourless solid, m.p. 138°-140° C. (decomposition)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 5.0 grams (0.025 moles) of phenacylbromide in 40 milliliters of acetone was mixed with a solution of 3.27 grams (0.025 moles) of 3,4,5,6-tetrahydro-5-methyl-s-triazin 2(1H)thione in 450 milliliters of acetone. 6-Hydroxy-3-methyl-6-phenyl-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide crystallized out as a colourless solid, m.p. 149°-150° C. (decomposition). The yield was 7.35 grams (89%). 6-Hydroxy-3-methyl-6-phenyl-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide crystallized out as a colourless solid, m.p. 149°-150° C. (decomposition)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-bromo-3-(m-nitrobenzoyl)propionic acid (7.55 g, 0.024 mole) in methanol (50 ml) was mixed with a solution of 5-methyl-3,4,5,6-tetrahydro-s-triazine-2(1H)thione (3.27 g, 0.025 mole) in the same solvent (170 ml). After 3 hours at room temperature the solvent was evaporated to small volume when a colourless solid crystallised, which was collected to give 7-carboxymethyl-6-hydroxy-3-methyl-6-(m-nitrophenyl)-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide methanolate (7.5 g), m.p. 144°-145° C. (decomposition). After 3 hours at room temperature the solvent was evaporated to small volume when a colourless solid crystallised which was collected

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-bromo-3-(p-chlorobenzoyl) propionic acid (7.29 g, 0.025 moles) in methanol (40 ml) was mixed with a solution of 5-methyl-3,4,5,6-tetrahydro-s-triazin-2(1H)-thione (3.27 g, 0.025 moles) in the same solvent (150 ml) and left for one hour. Evaporation of the solvent gave 7-carboxymethyl-6-(p-chlorophenyl)-6-hydroxy-3-methyl-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide as a pale yellow solid (9.6 g), m.p. 111°-113° C. Evaporation of the solvent

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-benzoyl-3-bromo-propionic acid (6.4 g, 0.025 moles) in methanol (30 ml) was mixed with a solution of 5-methyl-3,4,5,6-tetrahydro-s-triazine-2(1H)-thione (3.27 g, 0.025 moles) in the same solvent (100 ml) and left for 3 hours. Evaporation of the solvent gave 7-carboxymethyl-6-hydroxy-3-methyl-6-phenyl-3,4,6,7-tetrahydro-2H-thiazolo[3,2-a]-s-triazine hydrobromide quarter hydrate as a pale yellow solid (8.8 g), m.p. 74°-77° C. Evaporation of the solvent