HRID1787923

反应详情

EQUATION

反应方程式

HRID 1787923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring suspension of 4-(Boc-amino)pyridine-3-carboxylic acid (1.04 g, 4.37 mmol) in methanol (3.5 mL) was added a 2 M solution of (trimethylsilyl)diazomethane in hexanes (3.5 mL, 7 mmol). After 15 min, acetic acid was added and the solvents were removed in vacuo. The residue was chromatographed over silica gel, eluting with a step gradient of 20% ethyl acetate in hexanes through 70% ethyl acetate in hexanes. The product containing fractions were combined and concentrated in vacuo to give the title compound (0.894 g, 81%) as a white solid.

WORKUP

后处理

  1. customthe solvents were removed in vacuo
  2. customThe residue was chromatographed over silica gel
  3. washeluting with a step gradient of 20% ethyl acetate in hexanes through 70% ethyl acetate in hexanes
  4. additionThe product containing fractions
  5. concentrationconcentrated in vacuo