HRID1004324

反应详情

EQUATION

反应方程式

HRID 1004324 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

400 mg of tert-butyl 3-(ethoxycarbonyl)-4-[N-[(1RS,2RS)-2-(tert-butyldimethylsilyloxymethyl)-1-methyl-3-{5-(phenylcarbamoyl)-2-furyl}propyl]-N-(2-naphthylmethyl)carbamoyl]-4-methoxymethyloxy-3-butenoate prepared by the same reaction as in Example 1(2) by using N-(2-naphthylmethyl)-[(1RS,2RS)-2-(tert-butyldimethylsilyloxymethyl)-1-methyl-3-{5-(phenylcarbamoyl)-2-furyl}propyl]amine prepared in Reference Example 4 was dissolved in 4 ml of tetrahydrofuran and stirred together with 0.95 ml of 1.0M tetrabutylammonium fluoride in tetrahydrofuran solution at room temperature for 2 hours. The reaction solution was poured into water and extracted with ethyl acetate, and the organic layer was washed with saturated aqueous ammonium chloride and saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. The desiccant was filtered off, and the solvent was distilled off under reduced pressure. The residue was purified by column chromatography [hexane/ethyl acetate=1/1] to give 147 mg (yield: 43%) of the title compound as a colorless oily substance.

WORKUP

后处理

  1. customprepared in Reference Example 4
  2. extractionextracted with ethyl acetate
  3. washthe organic layer was washed with saturated aqueous ammonium chloride and saturated aqueous sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe desiccant was filtered off
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by column chromatography [hexane/ethyl acetate=1/1]