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HRID1597619

反应详情

EQUATION

反应方程式

HRID 1597619 的结构方程式

REACTANTS

反应物

2
结构：O=C(O)C(F)(F)F
HCID6422

未命名化合物

结构：CC(C)(C)OC(=O)[C@H](CNC(=O)CNC(=O)CCCc1csc(N)n1)NS(=O)(=O)c1ccccc1
HCID86754469

未命名化合物

PRODUCTS

生成物

1
结构：Nc1nc(CCCC(=O)NCC(=O)NC[C@H](NS(=O)(=O)c2ccccc2)C(=O)O)cs1
HCID15872149

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

Ester 1-8 (365 mg, 0.69 mmol) was dissolved in CH2Cl2 (3.5 mL), then TFA (3.5 mL) was added. After 5 h the reaction mixture was concentrated, azeotroped with toluene, then purified by sequential flash chromatography (silica, 22:20:1:1 EtOAc/EtOH/H2O/NH4OH, then silica, 4:1:1 CH2Cl2/MeOH/HOAc, then 7:1:1 CH2Cl2/MeOH/HOAc), providing 1-9 as a white solid.

WORKUP

后处理

  1. concentrationAfter 5 h the reaction mixture was concentrated
  2. customazeotroped with toluene
  3. custompurified by sequential flash chromatography (silica, 22:20:1:1 EtOAc/EtOH/H2O/NH4OH