HRID1643384
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Method B. (3S)-2-oxo-3-benzoylamino-5-acetoacetyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine-1-acetic acid benzyl ester (602g). A 0° C. solution of (3S)-2-oxo-3-(benzoylamino)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine-1-acetic acid benzyl ester (600b) (465 mg, 1.10 mmol) in CH2Cl2 (5 ml) was treated with acetoacetic acid in 1 ml of CH2Cl2 followed by slow addition of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (431 mg, 2.2 mmol) in 2 ml of CH2Cl2 under N2 atmosphere. After 15 min the reaction was poured onto EtOAc, washed with aq. 5% NaHSO4, dried over Na2SO4 and concentrated in vacuo.
WORKUP
后处理
- additionAfter 15 min the reaction was poured onto EtOAc
- washwashed with aq. 5% NaHSO4
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo