HRID523858

反应详情

EQUATION

反应方程式

HRID 523858 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 2-chlormethylphenylacetonitrile (200 mg, 1.21 mmol) and thiourea (101 mg, 1.33 mmol) were mixed in 1 ml of methanol. The mixture was heated to reflux for 3 to 4 hours. The reaction mixture was evaporated. After that, 1 ml of methanol and 4 ml of acetone were added and the mixture was stirred for one hour. The crystalline material was filtered and the product was dried under high vacuum overnight to yield 231 mg (0.95 mmol, yield 79%) of product as off white crystals, with purity greater than 95%. 1H NMR (300 MHz, d6-DMSO) δ 4.14 (s, 2H), 4.56 (s, 2H), 7.37 (m, 2H), 7.45 (m, 2H), 9.23 (s, 4H). (M+H) 205.97

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 3 to 4 hours
  3. customThe reaction mixture was evaporated
  4. additionAfter that, 1 ml of methanol and 4 ml of acetone were added
  5. filtrationThe crystalline material was filtered
  6. customthe product was dried under high vacuum overnight