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HRID23653

反应详情

EQUATION

反应方程式

HRID 23653 的结构方程式

REACTANTS

反应物

2
结构：c1ccc(P(c2ccccc2)c2ccccc2)cc1
HCID11776

Triphenylphosphine

C18H15P

结构：CN(Cc1sc2c(=O)c(C(=O)NCc3ccc(Cl)cc3)cn(C)c2c1CN=[N+]=[N-])C[C@@H](O)c1ccccn1
HCID59985226

未命名化合物

PRODUCTS

生成物

1
结构：CN(Cc1sc2c(=O)c(C(=O)NCc3ccc(Cl)cc3)cn(C)c2c1CN)C[C@@H](O)c1ccccn1
HCID59985219

未命名化合物

收率 78.6%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：C1CCOC1
催化剂HCID8028

Tetrahydrofuran

C4H8O

结构：O
溶剂HCID962

Water

H2O

PROCEDURE

实验过程

A solution of 111 mg of 3-(azidomethyl)-N-(4-chlorobenzyl)-2-{[[(2R)-2-hydroxy-2-pyridin-2-ylethyl](methyl)amino]methyl}-4-methyl-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide and 58 mg of triphenylphosphine in 2 mL of THF containing 5 drops of water is stirred overnight, then concentrated under reduced pressure with CHCl3/MeOH azeotrope. Flash chromatography on silica gel using 4-10% methanolic ammonia in CH2Cl2 provides 83.1 mg of the amine as a white solid. Recrystallization from acetonitrile furnishes white solid.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure with CHCl3/MeOH