반응 #56246

반응 방정식

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

수율 5.7%

용매

water

ethanol

ethanol

반응 조건

후처리

1. 1
   workup.ADDITIONwas treated with 1.5 g of activated carbon
2. 2
   여과was filtered
3. 3
   세척The filter was washed twice with 5 ml of a 9-1 ethanol-water mixture
4. 4
   workup.ADDITIONthe filtrate was added dropwise over 50 minutes
5. 5
   workup.STIRRINGwith stirring at room temperature to 80 ml of ethanol which
6. 6
   기타precipitation of the sodium salt
7. 7
   workup.STIRRINGThe mixture was stirred for 2 hours at 0° C.
8. 8
   여과filtered
9. 9
   세척The crystals were washed with ethanol
10. 10
    기타dried under reduced pressure

실험 절차

10 g of the syn isomer of 3-acetoxymethyl-7-[2-(2-amino-4-thiazolyl)-2-methoxyimino-acetamido]-ceph-3-eme-4-carboxylic acid containing 7.2% of ethanol were added to a solution of 2 g of sodium acetate in 7.5 ml of water and 20 ml of absolute ethanol and the mixture was stirred for 15 minutes, was treated with 1.5 g of activated carbon and was filtered. The filter was washed twice with 5 ml of a 9-1 ethanol-water mixture and the filtrate was added dropwise over 50 minutes with stirring at room temperature to 80 ml of ethanol which caused precipitation of the sodium salt. The mixture was stirred for 2 hours at 0° C. and was vacuum filtered. The crystals were washed with ethanol and dried under reduced pressure to obtain 8.45 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 5.7% of water.

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