HRID60532

反应详情

EQUATION

反应方程式

HRID 60532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Pyridine (0.6 g, 7.6 mmol) was added to 6-amino-2-{[(1S)-1-phenylethyl]thio}pyrimidin-4-ol (1 g, 4 mmol) and KSCN (1.7 g, 16 mmol) in DMF (20 mL). The reaction mixture was cooled to 0° C. and bromine (0.65 g, 4.0 mmol) was then added in one portion. The reaction mixture was poured into water after 2 h and the orange precipitate was filtered off and washed with water. The solid was suspended in a mixture of DMF (6 mL) and water (2 mL) and heated to 110° C. After 30 h, the reaction mixture was poured into water, the yellowish precipitate was filtered off and washed with water and ether. The solid was dried in vacuum at 40° C. to give the title compound (0.8 g, 65% yield).

WORKUP

后处理

  1. filtrationthe orange precipitate was filtered off
  2. washwashed with water
  3. additionThe solid was suspended in a mixture of DMF (6 mL) and water (2 mL)
  4. temperatureheated to 110° C
  5. additionthe reaction mixture was poured into water
  6. filtrationthe yellowish precipitate was filtered off
  7. washwashed with water and ether
  8. customThe solid was dried in vacuum at 40° C.