HRID881715

反应详情

EQUATION

反应方程式

HRID 881715 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

To a round bottom flask containing (8-(4-bromophenyl)-1,4-dioxaspiro[4.5]decan-8-yl)methanol (4.88 g, 14.91 mmol) was added acetone (34 ml) and water (17 ml) at room temperature. p-toluenesulfonic acid (57 mg, 0.30 mmol) was then added and the mixture heated to 75° C. for 1 hour. The content was cooled to room temperature and concentrated under reduced pressure to remove the excess acetone. The resulting aqueous mixture was extracted with EtOAc twice. The combined organic portion was dried over sodium sulfate and concentrated to afford the title compound as white solid. (4.22 g) LC/MS, ESI-MS: non-ionizable, RT: 1.05 (Condition E).

WORKUP

后处理

  1. temperatureThe content was cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. customto remove the excess acetone
  4. extractionThe resulting aqueous mixture was extracted with EtOAc twice
  5. dry with materialThe combined organic portion was dried over sodium sulfate
  6. concentrationconcentrated