HRID498242
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customprepared by the following procedure
- customthe precipitate was collected
- customdried
- temperatureby heating in MeOH (12 ml)/4N HCl-Et2O (3 ml) for 20 h at 40° C.
- customObtained as a yellow solid (1.36 g, crude product)