HRID1479854

反应详情

EQUATION

反应方程式

HRID 1479854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Compound 13A (645 mg, 2.36 mmol) dissolved in THF (10 ml) and water (5 ml) was added with LiOH.H2O (3 equiv., 297 mg) and the reaction was stirred at rt 3 hours. The reaction was concentrated under vacuum. Water was added and 10% HCl till precipitation of the acid. The acid was extracted with ethyl acetate and the organic phase was washed with Brine, dried over sodium sulfate and concentrated under vacuum to give 600 mg of 15C as a white solid. Yield=98%. 1HNMR (DMSO, 200 MHz) δ 1.38 (2H, m), 1.35 (2H, bs), 7.42 (2H, m), 7.80 (2H, m), 8.80 (1H, bs), 12.46 (1H, bs)

WORKUP

后处理

  1. concentrationThe reaction was concentrated under vacuum
  2. additionWater was added
  3. custom10% HCl till precipitation of the acid
  4. extractionThe acid was extracted with ethyl acetate
  5. washthe organic phase was washed with Brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under vacuum