HRID2086251

反应详情

EQUATION

反应方程式

HRID 2086251 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of tert-butyl 2-(Boc-L-methionyl)-1-hydrazine carboxylate methylsulfonium iodide (18 g) in DMF (200 ml) was combined with sodium hydride (3.93 g, in oil) with cooling on ice, and then stirred at room temperature for 3 hours The reaction mixture was combined with ice-water, and extracted with ethyl acetate, and the organic phase was washed with water and brine, dried and concentrated to obtain a residue, which was triturated from isopropyl ether/hexane (1/1) solution, collected by filtration, washed with isopropyl ether/hexane (1/1) solution and dried to obtain the title compound (5.7 g) as a colorless solid.

WORKUP

后处理

  1. temperaturewith cooling on ice
  2. extractionextracted with ethyl acetate
  3. washthe organic phase was washed with water and brine
  4. customdried
  5. concentrationconcentrated
  6. customto obtain a residue, which
  7. customwas triturated from isopropyl ether/hexane (1/1) solution
  8. filtrationcollected by filtration
  9. washwashed with isopropyl ether/hexane (1/1) solution
  10. customdried