反応 #74995

反応方程式

Rifamycin S

1-amino-4-methylpiperazine

1,3,5-trimethyl-hexahydro-1,3,5-triazine

rifamycin

paraformaldehyde

→

rifampicin

溶媒

acetic acid

dimethylformamide

反応条件

後処理

1. 1
   workup.WAITthe reaction is continued at 50° C. for about 1 hour until it

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.

出典