반응 #214080

반응 방정식

2-(2-carbobenzoxyamino-5-fluoro-4-thiazolyl)-2-methoxyiminoacetic acid

7β-amino-3-cephem-4-carboxylic acid diphenylmethyl ester

dicyclohexylcarbodiimide

→

7β-[2-(2-carbobenzoxyamino-5-fluoro-4-thiazolyl)-2-methoxyiminoacetamido]-3-cephem-4-carboxylic acid diphenylmethyl ester

수율 70.9%

용매

dichloromethane

반응 조건

후처리

1. 1
   농축concentrated
2. 2
   기타to remove dichloromethane
3. 3
   workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
4. 4
   여과filtered
5. 5
   기타to remove solid material
6. 6
   농축concentrated under reduced pressure
7. 7
   기타The resultant product is purified by silica gel column chromatography

실험 절차

To a solution of 2-(2-carbobenzoxyamino-5-fluoro-4-thiazolyl)-2-methoxyiminoacetic acid (207 mg) and 7β-amino-3-cephem-4-carboxylic acid diphenylmethyl ester (207 mg) in dichloromethane (20 ml) is added dicyclohexylcarbodiimide (142 mg), and the mixture is stirred at 23° C. for 60 minutes and concentrated to remove dichloromethane. The residue is dissolved in ethyl acetate, filtered to remove solid material, and concentrated under reduced pressure. The resultant product is purified by silica gel column chromatography to afford 7β-[2-(2-carbobenzoxyamino-5-fluoro-4-thiazolyl)-2-methoxyiminoacetamido]-3-cephem-4-carboxylic acid diphenylmethyl ester (281 mg).

출처