HRID1260502

反应详情

EQUATION

反应方程式

HRID 1260502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
240 °C

PROCEDURE

实验过程

N-[3-(4-Hydroxyphenyl)-1-methylpropyl]acetamide (104.9 mg, 0.51 mmol), 2-chloro-5-cyclopentyloxypyridine (100 mg, 0.51 mmol) and sodium hydride (50% in oil) (26 mg, 0.54 mmol) were treated at 230° C. in 5 ml of N-methylpyrrolidinone in a microwave reactor for 1 h. Addition of a further 26 mg of sodium hydride was followed by again heating at 240° C. for 1 h. The reaction mixture was concentrated, and the residue was taken up in ethyl acetate and water. The organic phase was separated off, concentrated and purified by preparative HPLC (PR18, acetonitrile/water 0.1% TFA). Yield: 16 mg (9%), M+H+: 369.17.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. customThe organic phase was separated off
  3. concentrationconcentrated
  4. custompurified by preparative HPLC (PR18, acetonitrile/water 0.1% TFA)