HRID1919899

反应详情

EQUATION

反应方程式

HRID 1919899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 4-{3-tert-butoxy-2-[(tert-butoxycarbonyl)amino]-3-oxopropyl}benzoate (0.40 g, 1.05 mmol) was dissolved in THF (10 mL). KOSiMe3 (0.27 g, 2.10 mmol) was added to the solution and allowed to stir overnight at room temperature under nitrogen. Saturated ammonium chloride was added and allowed to stir. Hydrochloric acid (2 mL, 1M solution) was added. The reaction was diluted with ethyl acetate and separated. The aqueous layer was extracted three times with ethyl acetate. The combined organic layer was dried with sodium sulfate, filtered, and concentrated. The resulting material was purified by HPLC. MS: cal'd 365 (MH+), exp 388 (MH+).

WORKUP

后处理

  1. stirringto stir
  2. customseparated
  3. extractionThe aqueous layer was extracted three times with ethyl acetate
  4. dry with materialThe combined organic layer was dried with sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe resulting material was purified by HPLC