HRID2230399

反应详情

EQUATION

反应方程式

HRID 2230399 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 (S)-3-[(2S,3R,4R,5S)-2,3,4,6-tetrahydroxy-5-(L-leucyl)aminohexanoyl]amino-3-phenylpropionic acid hydrochloride (1.84 g) in methanol (40 ml) was added a solution of diphenyldiazomethane (1.45 g) in methanol (20 ml) and the mixture was stirred at room temperature for 4 hours. After addition of acetic acid (0.1 ml), the reaction mixture was extracted with ethyl acetate. The extract was washed with aqueous sodium hydrogencarbonate solution and saturated brine respectively and the ethyl acetate solution was dried over anhydrous sodium sulfate. Removal of the organic solvent gave a residue, which was purified by silica gel column chromatography. Elution with ethyl acetate-methnaol (2:1) provided the title compound (2.05 g).

WORKUP

后处理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washThe extract was washed with aqueous sodium hydrogencarbonate solution and saturated brine respectively
  3. dry with materialthe ethyl acetate solution was dried over anhydrous sodium sulfate
  4. customRemoval of the organic solvent
  5. customgave a residue, which
  6. customwas purified by silica gel column chromatography
  7. washElution with ethyl acetate-methnaol (2:1)