HRID1039966

反应详情

EQUATION

反应方程式

HRID 1039966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product of Step 1 (3.0 g, 9.4 mmol) was dissolved in 30 mL of 1:1 THF:HCl (3N) and heated at 50° C. for 8 hours and the solution neutralized with solid KHCO3 and then EtOAc (100 mL) and water (20 mL) were added. The aqueous layer was then extracted with EtOAc (50 mL) and the combined organic layers were washed with brine (50 mL), evaporated to a slurry which was treated with hexanes (20 mL). Filtration and drying afforded 4-(5-bromo-1,3-thiazol-2-yl)-4-hydroxycyclohexanone as a white solid (2.1 g, 7.7 mmol).

WORKUP

后处理

  1. extractionThe aqueous layer was then extracted with EtOAc (50 mL)
  2. washthe combined organic layers were washed with brine (50 mL)
  3. customevaporated to a slurry which
  4. additionwas treated with hexanes (20 mL)
  5. filtrationFiltration
  6. customdrying