HRID1400498

反应详情

EQUATION

反应方程式

HRID 1400498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Trimethylsulfonium iodide (3.34 g, 16.3 mmol) was dissolved in DMF (20 mL) and stirred at RT for 5 min. Sodium hydride (600 mg, 25 mmol) was added portionwise at the same temperature and stirred for 15 min. 4-Acetyl pyrimidine (1 g, 8.1 mmol) in 0.5 mL DMSO was added dropwise and the reaction mixture stirred for 1 h. After completion of reaction, the mixture was poured into ice-cold water and extracted with Ether (3×). The combined organic layer was washed with water several times followed by brine, and dried over sodium sulfate, then evaporated to provide 600 mg of 4-(2-Methyl-oxiranyl)-pyrimidine. 1H NMR (CDCl3, freebase) δ (ppm): 9.15 (s, 1H), 8.7 (d, 1H), 7.35 (d, 1H), 2.95 (d, 1H), 2.88 (d, 1H), 1.8 (s, 3H).

WORKUP

后处理

  1. stirringstirred for 15 min
  2. stirringthe reaction mixture stirred for 1 h
  3. customAfter completion of reaction
  4. additionthe mixture was poured into ice-cold water
  5. extractionextracted with Ether (3×)
  6. washThe combined organic layer was washed with water several times
  7. dry with materialdried over sodium sulfate
  8. customevaporated