反应 #1876830
ord-c7cdb97a3cc049f6887ac3a666b6ecef
反应方程式
Boc-D-Pal
Benzyl bromide
→
Boc-D-Pal(Bzl) Hydrobromide
收率 85.0%
试剂
无
反应条件
温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他A cleasr solution resulted
- 2其他A white precipitate formed
- 3workup.WAITTLC after 17 hours showed
- 4workup.STIRRINGstirring
- 5其他continued for a total of 5 days, when
- 6其他The solvent was evaporated under reduced pressure
- 7其他the residue recrystallized from EtOH/ethyl acetate
实验过程
Boc-D-Pal (1.36 g, 6.0 mmol) was suspended in 60 ml of acetonitrile. Benzyl bromide (about 50 mmol) was added and the mixture was warmed to 50° C. on a water bath. A cleasr solution resulted, and was stirred at room temperature for 16 hours. A white precipitate formed; TLC after 17 hours showed some starting remaining starting material; stirring continued for a total of 5 days, when the reaction was complete. The solvent was evaporated under reduced pressure, and the residue recrystallized from EtOH/ethyl acetate. Yield: 85%; m.p. 166–170° C.