HRID129009

反应详情

EQUATION

反应方程式

HRID 129009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl 3-(4-chloro-6-methyl-2-methoxymethylpyrimidin-5-yl)propionate (3.6 g, 0.013 mol), 4-bromobenzylamine hydrochloride (3.0 g, 0.013 mol), NaHCO3 (2.4 g, 0.028 mol), and nBuOH (25 mL) was heated under reflux for 24 h. The mixture was concentrated, taken up in water, and extracted with CH2Cl2. The combined extracts were dried (MgSO4) and concentrated to give a brown oil. Purification by flash chromatography (5% MeOH/CH2Cl2) gave 3.6 g (72%) of product as an off-white solid, mp 64°-66° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 24 h
  3. concentrationThe mixture was concentrated
  4. extractionextracted with CH2Cl2
  5. dry with materialThe combined extracts were dried (MgSO4)
  6. concentrationconcentrated
  7. customto give a brown oil
  8. customPurification by flash chromatography (5% MeOH/CH2Cl2)