HRID1159673

反应详情

EQUATION

反应方程式

HRID 1159673 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-(4-nitrophenyl)ethanimidamide hydrochloride (0.22 g, 1.0 mmol), dimethyl acetyl-succinate (0.19 g, 1.0 mmol), and sodium methoxide (0.07 g, 1.3 mmol) in MeOH (10 mL) was refluxed for 15 hours. After cooling to room temperature, the separated solids were collected by suction and added to a pre-formed solution of thionyl chloride (0.65 mL, 8.9 mmol) in MeOH (7.5 mL). The resulting mixture was refluxed for 16 hours and then cooled to room temperature. Acetone was added and the precipitated solids were collected by suction, rinsed with acetone and dried under high vacuum for 4 hours to give methyl [4-hydroxy-6-methyl-2-(4-nitrobenzyl)-pyrimidin-5-yl]acetate (0.12 g, 38% yield) as a white solid.

WORKUP

后处理

  1. temperaturewas refluxed for 15 hours
  2. customthe separated solids were collected by suction
  3. temperatureThe resulting mixture was refluxed for 16 hours
  4. temperaturecooled to room temperature
  5. customthe precipitated solids were collected by suction
  6. washrinsed with acetone
  7. customdried under high vacuum for 4 hours