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HRID547274

反应详情

EQUATION

反应方程式

HRID 547274 的结构方程式

REACTANTS

反应物

3
结构：[H-].[Na+]
HCID24758

Sodium hydride

HNa

结构：CC(C)(C)OC(=O)CCN.Cl
HCID16218890

tert-Butyl beta-alaninate--hydrogen chloride (1/1)

C7H16ClNO2

结构：CC(=O)c1ccc(CBr)c(Cl)n1
HCID86011816

Ethanone, 1-[5-(bromomethyl)-6-chloro-2-pyridinyl]-

C8H7BrClNO

PRODUCTS

生成物

1
结构：CC(=O)c1ccc(CNCCC(=O)OC(C)(C)C)c(Cl)n1
HCID86595998

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

2 次

PROCEDURE

实验过程

To a solution of 3-amino-propionic acid tert-butyl ester hydrochloride (1.5 eq) in DMF is added NaH (3.5 eq). The resulting mixture is stirred at room temperature for 15 minutes and a solution of 1-(5-bromomethyl-6-chloro-pyridin-2-yl)-ethanone (1 eq) in DMF is then added. After stirring for 3 hours, it is partitioned with 20% EtOAc/hexane and H2O. The organic layer is washed with brine and dried. After concentration, 3-[(6-acetyl-2-chloro-pyridin-3-ylmethyl)-amino]-propionic acid tert-butyl ester is isolated by flash column chromatography. MS: (ES+): 313.1 (M+1)+.

WORKUP

后处理

  1. stirringAfter stirring for 3 hours
  2. customit is partitioned with 20% EtOAc/hexane and H2O
  3. washThe organic layer is washed with brine
  4. customdried
  5. concentrationAfter concentration