1,3,5-trimethyl-1,3,5-triazinane

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

実験手順: 7 g. Rifamycin S are dissolved in 25 ml. dimethylformamide, then, while stirring, there are successively added 2.4 g. acetic acid, 0.6 g. paraformaldehyde and 0.85 g. 1,3,5-trimethyl-hexahydro-1,3,5-triazine. The mixture is then kept at 50° C. for 3 hours until the reaction is completed, with the formation of 3-methyl-1,3-oxazino (5,6-c) rifamycin (thin layer chromatography on silica gel 60 F254 - Merck: blue spot at Rf 0.19, eluent chloroform:methanol 9:1 v/v). 3.1 g. 1-amino-4-methylpiperazine are then added and the reaction is continued at 50° C. for about 1 hour until it is completed, as demonstrated by the disappearance of the blue spot in the TLC. After treatment in the usual way, a high yield (7.2 g.) of rifampicin is obtained. It can easily be purified by crystallisation from acetone. the reaction is continued at 50° C. for about 1 hour until it

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

実験手順: 7 g. Rifamycin S are dissolved in 25 ml. dimethylformamide, then, while stirring, there are successively added 2.4 g. acetic acid, 0.6 g. paraformaldehyde and 0.85 g. 1,3,5-trimethyl-hexahydro-1,3,5-triazine. The mixture is then kept at 50° C. for 3 hours until the reaction is completed, with the formation of 3-methyl-1,3-oxazino (5,6-c) rifamycin (thin layer chromatography on silica gel 60 F254 - Merck: blue spot at Rf 0.19, eluent chloroform:methanol 9:1 v/v). 3.1 g. 1-amino-4-methylpiperazine are then added and the reaction is continued at 50° C. for about 1 hour until it is completed, as demonstrated by the disappearance of the blue spot in the TLC. After treatment in the usual way, a high yield (7.2 g.) of rifampicin is obtained. It can easily be purified by crystallisation from acetone. the reaction is continued at 50° C. for about 1 hour until it

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

実験手順: 7 g. Rifamycin S are dissolved in 25 ml. dimethylformamide, then, while stirring, there are successively added 2.4 g. acetic acid, 0.6 g. paraformaldehyde and 0.85 g. 1,3,5-trimethyl-hexahydro-1,3,5-triazine. The mixture is then kept at 50° C. for 3 hours until the reaction is completed, with the formation of 3-methyl-1,3-oxazino (5,6-c) rifamycin (thin layer chromatography on silica gel 60 F254 - Merck: blue spot at Rf 0.19, eluent chloroform:methanol 9:1 v/v). 3.1 g. 1-amino-4-methylpiperazine are then added and the reaction is continued at 50° C. for about 1 hour until it is completed, as demonstrated by the disappearance of the blue spot in the TLC. After treatment in the usual way, a high yield (7.2 g.) of rifampicin is obtained. It can easily be purified by crystallisation from acetone. the reaction is continued at 50° C. for about 1 hour until it

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 4.25 g (18.5 mmol) rac-4-cyclohexyl-4-nitro-butyric acid methyl ester were added 4.56 ml (32.5 mmol) 1,3,5-trimethylhexahydro-1,3,5-triazine and the mixture heated to 100° C. for 4 hours. The reaction mixture was cooled to ambient temperature and adsorbed on silica gel which was transferred on top of a silica gel column and purified by flash-chromatography with a gradient of heptane and 10 to 75% ethyl acetate: 2.55 g of title compound were isolated as colourless oil: MS (m/e): 240 (MH+). The reaction mixture was cooled to ambient temperature purified by flash-chromatography with a gradient of heptane and 10 to 75% ethyl acetate

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

実験手順: To the solution 19.5 g of 1,3,5-trimethylhexahydro-1,3,5-triazine in 20 ml of actonitrile and 150 ml of toluene, was slowly added 19 ml of chlorotrimethylsilane, which was then stirred for 10 min. 10 g of 1,2,3,9-tetrahydro-9-methyl-4H-carbazol-4-one and 8.2 g of 2-methyl imidazole was subsequently added to the reaction mixture, which was then stirred under reflux. After completion of reaction, the reaction mixture was evaporated, and then 200 ml of water was added to the resulting residue, which was then stirred for 2 hours at room temperature. The resulting solid was filtered and washed with water to give 7.95 g of light yellow title compound (yield 54%). was then stirred under reflux After completion of reaction the reaction mixture was evaporated 200 ml of water was added to the resulting residue, which was then stirred for 2 hours at room temperature The resulting solid was filtered washed with water

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

実験手順: 300 ml. of acetonitrile, 12.9 g. (0.1 mole) of 1,3,5-trimethylhexahydro-s-triazine; 43.8 g. (0.3 mole) of tert.-octylthiomethylamine and 12 g. of hydrogen chloride gas are reacted together in the manner of Example I. A yield of 43.7 g. (64.6% of theory) of the title compound is obtained.

反応条件: temp:-30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Two hundred ml. of acetonitrile and 6.45 g. (0.05 mole) of 1,3,5-trimethylhexahydro-s-triazine are charged to a 500 ml. 3-neck round bottom flask equipped with a stirrer, thermometer and dropping funnel. The mixture is stirred and cooled to -30° C. with a dry ice/acetone bath. Six grams of hydrogen chloride gas are added, followed by slow addition of 13.5 g. (0.15 mole) of tert.-butyl mercaptan dissolved in 50 ml. of acetonitrile. The mixture is then allowed to warm to room temperature and stand overnight. 3-neck round bottom flask equipped with a stirrer followed by slow addition of 13.5 g to warm to room temperature