HRID639311

反应详情

EQUATION

反应方程式

HRID 639311 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

A mixture of 0.12 g (0.4 mmol) 6-bromo-5-piperidin-1-yl-pyrazine-2-carboxylic acid methyl ester, 0.029 g (0.4 mmol) cyclopropyl methanol and 0.018 g (0.41 mmol) NaH (55% suspension in oil) in 2 mL DMF was shaken for an extended period of time. Afterwards, 0.1 mL KOH (5N aq.) was added and the mixture was heated to 45° C. for 1 h. After addition of formic acid the mixture was subjected to purification by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile, water and formic acid. The combined product fractions were evaporated to yield 11 mg (10%) of the title compound. m/z (ES+): 278.1 (M+H).

WORKUP

后处理

  1. customwas subjected to purification by preparative HPLC on reversed phase
  2. washeluting with a gradient
  3. customformed from acetonitrile, water and formic acid
  4. customThe combined product fractions were evaporated