HRID1880352

反应详情

EQUATION

反应方程式

HRID 1880352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of semicarbazide HCl (61.2 g, 534 mmol), ethyl-methyl ketone (35 g, 0.49 mol) in water (525 mL), sodium acetate (79.7 g, 972 mmol) was added at room temperature and maintained for 18 hours. The reaction mixture was filtered, the obtained solid was washed with ether (2×25 mL) and dried at 70° C. for 20 hours to afford butan-2-one semicarbazone (45 g, 72%) as white solid. 1H NMR (CDCl3) δ 7.9 (br, 1H), 5.0-6.0 (br, 2H), 2.3 (q, 2H), 1.82 (s, 3H), 1.1 (t, 3H).

WORKUP

后处理

  1. temperaturemaintained for 18 hours
  2. filtrationThe reaction mixture was filtered
  3. washthe obtained solid was washed with ether (2×25 mL)
  4. customdried at 70° C. for 20 hours