HRID415363

反应详情

EQUATION

反应方程式

HRID 415363 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

KSCN (10.76 g, 110.7 mmol) and pyridine (3.9 mL, 49.2 mmol) was added to 6-amino-2-{[(1S)-1-(2-fluorophenyl)ethyl]thio}pyrimidin-4-ol (6.53 g, 24.6 mmol) in DMF (70 mL). The mixture was cooled to 0° C. and Br2 was added dropwise. After 3.5 h the reaction mixture was poured into water and the formed precipitate was collected by filtration. The solid was suspended in a mixture of DMF (75 mL) and water (15 mL) and heated to 120° C. for 8 h. The reaction mixture was poured into water and the solid was collected by filtration and dried in vacuo at 40° C. to give the title compound (6.42 g, 81% yield).

WORKUP

后处理

  1. filtrationthe formed precipitate was collected by filtration
  2. additionThe solid was suspended in a mixture of DMF (75 mL) and water (15 mL)
  3. temperatureheated to 120° C. for 8 h
  4. additionThe reaction mixture was poured into water
  5. filtrationthe solid was collected by filtration
  6. customdried in vacuo at 40° C.