HRID2246225

反应详情

EQUATION

反应方程式

HRID 2246225 的结构方程式

PROCEDURE

实验过程

The process is performed as described in Example 1 (step 1.2.). Starting with 0.95 g (3.70 mmol) of 1-(5-bromo-2-pyridyl)-1,4-diazepane, obtained in step 11.2., and 0.94 g (3.70 mmol) of 2-(methylamino)-2-oxoethyl 4-nitrophenyl carbonate, prepared in step 2.2. of Example 2, and after chromatography on silica gel, eluting with a 30/70 mixture of ethyl acetate and cyclohexane and then with a 95/5 mixture of dichloromethane and methanol, followed by crystallization from diisopropyl ether, 0.97 g of product is obtained in the form of a white solid.

WORKUP

后处理

  1. customobtained in step 11.2
  2. washof Example 2, and after chromatography on silica gel, eluting with a 30/70 mixture of ethyl acetate and cyclohexane
  3. additionwith a 95/5 mixture of dichloromethane and methanol
  4. customfollowed by crystallization from diisopropyl ether