反応 #56247

反応方程式

formate

3-acetoxymethyl-7-[2-(2-amino-4-thiazolyl)-2-methoxyimino-acetamido]-ceph-3-eme-4-carboxylic acid

sodium acetate

→

sodium 3-acetoxymethyl-7-[2-(2-amino-4-thiazolyl)-2-methoxyimino-acetamido]-ceph-3-eme-4-carboxylate

収率 0.9%

溶媒

water

ethanol

反応条件

後処理

1. 1
   ろ過the mixture was filtered
2. 2
   workup.ADDITIONThe filtrate was added dropwise over one hour
3. 3
   workup.STIRRINGthe resulting mixture was stirred at room temperature for 3 hours and at 0° C. for 16 hours
4. 4
   ろ過filtered
5. 5
   洗浄the crystals were washed with ethanol
6. 6
   その他dried under reduced pressure

実験手順

10 g of the formate solvate of the syn isomer of 3-acetoxymethyl-7-[2-(2-amino-4-thiazolyl)-2-methoxyimino-acetamido]-ceph-3-eme-4-carboxylic acid (described in Belgium Pat. No. 850,662) were added at room temperature to a solution of 3.5 g of sodium acetate in 5 ml of water and 300 ml of ethanol and when dissolution was complete, the mixture was filtered. The filtrate was added dropwise over one hour with stirring at room temperature to 160 ml of absolute ethanol and the resulting mixture was stirred at room temperature for 3 hours and at 0° C. for 16 hours. The mixture was vacuum filtered and the crystals were washed with ethanol and dried under reduced pressure to obtain 7.75 g of the crystalline D form of the syn isomer of sodium 3-acetoxymethyl-7-[2-(2-amino-4-thiazolyl)-2-methoxyimino-acetamido]-ceph-3-eme-4-carboxylate containing 0.95% of water.

出典