HRID2170319

反应详情

EQUATION

反应方程式

HRID 2170319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-bromo-N-methoxy-N-methyl-2-(methylthio)pyrimidine-4-carboxamide (11A, 8.2 g, 28 mmol) in THF (120 mL) was added dropwise to a suspension of lithium aluminum hydride (1.06 G, 28 mmol) and THF (120 mL) at −78° C. The mixture was stirred for 10 minutes after addition finish. H2O (1.06 mL), 15% aqueous NaOH solution (1.06 mL) and H2O (3.18 mL) were successively added to the mixture at 0° C. very slowly. The resulting precipitate was filtered and washed with THF. The filtrate was concentrated in vacuo to afford crude of the title compound. MS (m/z): 233.14, [M+H]+.

WORKUP

后处理

  1. additionafter addition finish
  2. filtrationThe resulting precipitate was filtered
  3. washwashed with THF
  4. concentrationThe filtrate was concentrated in vacuo