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HRID276770

反应详情

EQUATION

反应方程式

HRID 276770 的结构方程式

REACTANTS

反应物

3
结构：Cl
HCID313

Hydrochloric Acid

ClH

结构：CCOC(C)=O
HCID8857

Ethyl acetate

C4H8O2

结构：CC(C)C[C@H](NC(=O)[C@H](CO)NC(=O)[C@H](CCC(N)=O)NC(=O)CNC1CCCCC1)C(=O)OCc1ccccc1
HCID69994320

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)C[C@H](NC(=O)[C@H](CO)NC(=O)[C@H](CCC(N)=O)NC(=O)CNC1CCCCC1)C(=O)OCc1ccccc1.Cl
HCID69994356

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CO
溶剂HCID887

Methanol

CH4O

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

The N-(cyclohexylglycyl-glutaminyl-serinyl)leucine benzyl ester (SEQ ID NO:3) hydrochloride (1.478 Kg) was slurried in methanol (14.8 L) at room temperature and the batch stirred for 1 hr. Ethyl acetate (29.6 L) was added over 30 minutes, the batch was cooled to 0-5° C. and aged for an hour. The solid collected by filtration, washed with cold (0-5° C.) methanol/ethyl acetate (4.5 L, 1:2), dried on the filter for 45 minutes, under nitrogen, and then dried under vacuum, at 40° C. This material was then utilized in subsequent reactions.

WORKUP

后处理

  1. filtrationThe solid collected by filtration
  2. washwashed with cold (0-5° C.) methanol/ethyl acetate (4.5 L, 1:2)
  3. customdried on the
  4. filtrationfilter for 45 minutes, under nitrogen
  5. customdried under vacuum, at 40° C