HRID872197

反应详情

EQUATION

反应方程式

HRID 872197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium borohydride (0.24 g) is added to an ice-cold solution of 4-[2-(5-bromo-2-chloro-pyridin-4-yl)-acetyl]-piperidine-1-carboxylic acid tert-butyl ester (1.65 g) in tetrahydrofuran (40 mL) and water (10 mL). The resulting mixture is stirred for 0.5 h. 2 N aqueous citric acid solution is added and the mixture is extracted with ethyl acetate. The combined extracts are washed with aqueous NaHCO3 solution and brine, dried (MgSO4), and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 65:35) to give the title compound. Mass spectrum (ESI+): m/z=419/421/423 (Cl+Br) [M+H]+.

WORKUP

后处理

  1. extractionthe mixture is extracted with ethyl acetate
  2. washThe combined extracts are washed with aqueous NaHCO3 solution and brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 65:35)