HRID1258606

反应详情

EQUATION

反应方程式

HRID 1258606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of tert-butyl (6-formylpyridin-2-yl)carbamate (13.46 g, 60.57 mmol, 1 eq.) in 200 ml of THF cooled dot 0° C. was added NaBH4 (2.29 g, 60.57 mmol, 1 eq.) portion wise. The reaction was stirred at 0° C. for 1 h and quenched with sat. aqueous NH4Cl. The aqueous layer was extracted with DCM and the organics were combined, dried over MgSO4 and concentrated. The crude residue was purified by chromatography on silica gel to give tert-butyl [6-(hydroxymethyl)pyridin-2-yl]carbamate (9.95 g, 70% yield over 2 steps) as a clear viscous oil.

WORKUP

后处理

  1. customquenched with sat. aqueous NH4Cl
  2. extractionThe aqueous layer was extracted with DCM
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe crude residue was purified by chromatography on silica gel