HRID386607

反应详情

EQUATION

反应方程式

HRID 386607 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

To a stirred solution of ethyl[[3-(benzyloxy)-2,2-dimethylpropanoyl](phenyl)amino]acetate from Step C (530. mg, 1.44 mmol) in THF (10 mL), at ambient temperature, was added aqueous 1M NaOH (2.40 mL, 2.40 mmol). The stirred reaction was then heated to 50° C. for 19 hours, before being allowed to cool to ambient temperature. The bulk of the THF was then removed in vacuo, and aqueous 1M HCl (2.4 mL, 2.4 mmol) was then added resulting in an oily biphasic mixture. The mixture was extracted with ethyl acetate (twice) and the combined organics were washed with water and lastly saturated brine. The organics were then dried over sodium sulfate, filtered and concentrated in vacuo to yield the title compound which was used without further purification. MS: m/z=342 (M+1).

WORKUP

后处理

  1. customThe stirred reaction
  2. temperatureto cool to ambient temperature
  3. additionwas then added
  4. customresulting in an oily biphasic mixture
  5. extractionThe mixture was extracted with ethyl acetate (twice) and the combined
  6. washorganics were washed with water and lastly saturated brine
  7. dry with materialThe organics were then dried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo