HRID656989

反应详情

EQUATION

反应方程式

HRID 656989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 1,1-dimethylethyl {1-[2-(7-fluoro-2-oxo-1(2H)-quinoxalinyl)ethyl]-4-piperidinyl}carbamate (8.72 g, 22.36 mmol) in methanol (90 ml) and dichloromethane (150 mL) was treated with 4 M hydrogen chloride in 1,4-dioxane (150 mL) (added in a slow stream, some exotherm and rapid precipitation observed) and stirred at room temperature for 2.5 h. The mixture was evaporated to dryness and the residue was triturated with ether. The solid was filtered off, washed with ether and dried to give the amine salt as a grey-green solid (8.06 g, 99%).

WORKUP

后处理

  1. additionadded in a slow stream
  2. customsome exotherm and rapid precipitation
  3. customThe mixture was evaporated to dryness
  4. customthe residue was triturated with ether
  5. filtrationThe solid was filtered off
  6. washwashed with ether
  7. customdried