反応 #1543046

反応方程式

Boc-D-Pal

Benzyl bromide

→

Boc-D-Pal(Bzl) Hydrobromide

収率 85.0%

溶媒

acetonitrile

反応条件

後処理

1. 1
   その他A clear solution resulted
2. 2
   その他A white precipitate formed
3. 3
   workup.WAITTLC after 17 hours showed
4. 4
   workup.STIRRINGstirring
5. 5
   その他continued for a total of 5 days, when
6. 6
   その他The solvent was evaporated under reduced pressure
7. 7
   その他the residue recrystallized from EtOH/ethyl acetate

実験手順

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 clear 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.

出典