HRID591276

反应详情

EQUATION

反应方程式

HRID 591276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 54 mg 1-fluoro-2-iodoethane (0.31 mmol) in N,N-dimethylformamide (10 mL) was subsequently added 101 mg potassium carbonate (0.73 mmol), followed by 100 mg di-tert-butyl (2S)-2-[(tert-butoxycarbonyl)amino]-5-(4-hydroxybenzyl)-hexanedioate (from example 12d; 0.21 mmol), and the resulting mixture was stirred for 4 h at room temperature. The mixture was then partitioned between water and ethyl acetate, the aqueous layer was than extracted with ethyl acetate again. The combined organic layers were washed with brine, dried over sodium sulfate, and evaporated. The residue was purified by preparative HPLC, method A to give 85 mg (62% purity adjusted yield) of the target compound in approx. 80% purity.

WORKUP

后处理

  1. customThe mixture was then partitioned between water and ethyl acetate
  2. extractionthan extracted with ethyl acetate again
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customThe residue was purified by preparative HPLC, method A
  7. customto give
  8. custom85 mg (62% purity adjusted yield) of the target compound in approx. 80% purity