HRID498242

反应详情

EQUATION

反应方程式

HRID 498242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
155 °C

PROCEDURE

实验过程

The title compound was prepared from 3-(2-methyl-pyrimidin-4-yl)-benzoic acid methyl ester [prepared by the following procedure: A mixture of 3-acetyl-benzoic acid (0.82 g, 5 mmol), N-(bis-acetylamino-methyl)-acetamide (0.94 g, 5 mmol) and conc. H2SO4 (0.01 ml) was heated to 155° C. for 6 h. The cooled mixture was diluted with H2O (20 ml) and the precipitate was collected, dried and esterified by heating in MeOH (12 ml)/4N HCl-Et2O (3 ml) for 20 h at 40° C.; white crystals (0.27 g).] (0.80 g, 3.5 mmol by treatment with lithium tert-butyl acetate according to general procedure K (method b). Obtained as a yellow solid (1.36 g, crude product).

WORKUP

后处理

  1. customprepared by the following procedure
  2. customthe precipitate was collected
  3. customdried
  4. temperatureby heating in MeOH (12 ml)/4N HCl-Et2O (3 ml) for 20 h at 40° C.
  5. customObtained as a yellow solid (1.36 g, crude product)