HRID1284042

反应详情

EQUATION

反应方程式

HRID 1284042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

51 g Nε-tert.butyloxycarbonyl-L-lysine were converted in a conventional manner into the benzyltriethylammonium salt and then stirred in 700 ml dimethylformamide with 81 g benzyloxycarbonyl-L-asparagine-4-nitrophenyl ester with the addition of 1 equivalent of pyridine for 48 hours at 20°. The residue left after vacuum evaporation was treated with ethyl acetate and potassium hydrogen sulfate solutions simultaneously; the thick precipitate formed was filtered off and then recrystallised from ethanol/petroleum ether. F = 174° - 175° (Z);[α]D20 = + 13.8° (c = 1.0; in pyridine). Yield = 70 g (71 % of the theoretical amount).

WORKUP

后处理

  1. waitThe residue left
  2. customafter vacuum evaporation
  3. additionwas treated with ethyl acetate and potassium hydrogen sulfate solutions simultaneously
  4. customthe thick precipitate formed
  5. filtrationwas filtered off
  6. customrecrystallised from ethanol/petroleum ether
  7. customF = 174° - 175° (Z)
  8. custom[α]D20 = + 13.8° (c = 1.0; in pyridine)