HRID1009001

反应详情

EQUATION

反应方程式

HRID 1009001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 5-methyl-benzo[b]thiophenesulfonyl chloride (Maybridge, CAS: 90273-30-6, 0.37 g) in acetonitrile (5.0 mL) were added sodium cyanate (0.163 g) in one portion and pyridine (0.60 mL). The reaction mixture was stirred at rt for 3 h, then 2-amino-5-bromothiazole hydrobromide (0.286 g) was added in one portion. The mixture was stirred at rt for 4 h and quenched with 70% acetic acid (2.4 mL) and water (4.0 mL). The suspension was filtered, washed with waterlethanol and water, dried over P2O5 under high vacuum to obtain the desired compound (0.372 g) as a creamy solid. MS (ISN): m/e 430.1, 432.0 (M−H)−

WORKUP

后处理

  1. stirringThe mixture was stirred at rt for 4 h
  2. customquenched with 70% acetic acid (2.4 mL) and water (4.0 mL)
  3. filtrationThe suspension was filtered
  4. washwashed with waterlethanol and water
  5. dry with materialdried over P2O5 under high vacuum