反应 #1365715

反应方程式

H-Leu-OBzl

Z-Asp(OtBu)-OH

N-methyl-morpholine

isobutyl chloroformate

→

Z-Asp(OtBu)-Leu-OBzl

溶剂

triethylamine

THF

反应条件

后处理

1. 1
   过滤After filtering off the salt
2. 2
   浓缩the filtrate was concentrated to an oil
3. 3
   workup.DISSOLUTIONThe oil was dissolved in 100 mL of ethyl acetate
4. 4
   洗涤washed with 0.2 N HCl, 5% NaHCO3 and sat. NaCl
5. 5
   干燥dried over Na2SO4
6. 6
   过滤After filtration
7. 7
   其他the solvent was evaporated

实验过程

Z-Asp(OtBu)-OH (10.23 g) in THF (50 mL) was added N-methyl-morpholine (3.30 mL) and isobutyl chloroformate (3.90 mL) at −20° C. After 10 min, the reaction mixture was added to the solution of H-Leu-OBzl (11.81 g in 50 mL HCl3) at −20° C., followed by addition of triethylamine (4.18 mL); The resulting mixture was allowed to warm to room temp. After filtering off the salt, the filtrate was concentrated to an oil. The oil was dissolved in 100 mL of ethyl acetate; washed with 0.2 N HCl, 5% NaHCO3 and sat. NaCl; dried over Na2SO4. After filtration, the solvent was evaporated to give Z-Asp(OtBu)-Leu-OBzl as an oil of 14.81 g.

来源