HRID45187

反应详情

EQUATION

反应方程式

HRID 45187 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.22 g of {1-[8-(4-fluoro-phenyl)-1,4-dioxa-spiro[4.5]dec-8-yl]-butyl}-carbamic acid tert-butyl ester (16) were dissolved in 42 mL of acetone and 3 mL of 1N hydrochloric acid were added. The mixture was stirred at room temperature until conversion was complete. 40 mL of saturated aqueous sodium bicarbonate solution were added and the reaction mixture was extracted with ethyl acetate three times. The combined organic layer was extracted with brine, dried over sodium sulphate and evaporated to dryness to give 966 mg of crude (17), that was sufficiently pure for further conversion. Rt=1.72 min (Method 5). Detected mass: 308.2 (M-Isobutene+H+).

WORKUP

后处理

  1. extractionthe reaction mixture was extracted with ethyl acetate three times
  2. extractionThe combined organic layer was extracted with brine
  3. dry with materialdried over sodium sulphate
  4. customevaporated to dryness