HRID901027

反应详情

EQUATION

反应方程式

HRID 901027 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

47.2 To a stirred suspension of 3.9 g (4-{2-[4-(1-methyl-piperidin-4-yl)-piperazin-1-yl]-2-oxo-ethyl}-thiazol-2-yl)-carbamic acid tert-butyl ester was added 40 ml of 33% HBr in acetic acid. The reaction mixture was stirred at r.t. for 4 h. The mixture was left overnight in the fridge. Then it was concentrated to leave an off-white solid which was suspended in 50 ml Et2O, triturated and stirred at r.t. for 3 h. The product was collected by filtration, washed with Et2O and dried to give 5.6 g 2-(2-amino-thiazol-4-yl)-1-[4-(1-methyl-piperidin-4-yl)-piperazin-1-yl]-ethanone trihydrobromide. Off-white solid. MS 324.4 ([M+H]+)

WORKUP

后处理

  1. waitThe mixture was left overnight in the fridge
  2. concentrationThen it was concentrated
  3. customto leave an off-white solid which
  4. customtriturated
  5. stirringstirred at r.t. for 3 h
  6. filtrationThe product was collected by filtration
  7. washwashed with Et2O
  8. customdried