HRID410453

反应详情

EQUATION

反应方程式

HRID 410453 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

The product of Step 1 (60.5 g, 251 mmol) was diluted with DMF (5 mL). To this solution, NBS (49.1 g, 276 mmol) was added. The reaction was heated to 50° C. for 2 h. The reaction was cooled to 45° C. and H2O (600 mL) containing Na2SO3 (15.8 g, 125 mmol) was added drop wise. The reaction was stirred at room temperature for 1 h then filtered and washed with H2O (2×, 300 mL). The filtrate was dried under nitrogen to afford 8-(5-bromo-1,3-thiazol-2-yl)-1,4-dioxaspiro[4.5]decan-8-ol (68.15 g, 213 mmol, 85% yield).

WORKUP

后处理

  1. temperatureThe reaction was cooled to 45° C.
  2. additionwas added drop wise
  3. filtrationthen filtered
  4. washwashed with H2O (2×, 300 mL)
  5. customThe filtrate was dried under nitrogen