反応 #1683

反応方程式

trifluoroacetic acid

Boc-D-Phe-Pro-OBn

anisole

→

white powder

収率 85.0%

D-Phe-Pro-OBn.TFA

収率 85.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他the solvents were evaporated in vacuo
2. 2
   workup.DISSOLUTIONthe thick oily residue was dissolved in diethyl ether (1.5 L)
3. 3
   その他(72 hours)
4. 4
   ろ過The white precipitate was filtered
5. 5
   洗浄washed with diethyl ether (300 mL)
6. 6
   その他dried

実験手順

To a stirring solution of Boc-D-Phe-Pro-OBn (68 g, 150 mmol) in dichloromethane (50 mL) at 0° C., was added anisole (20 mL) followed by trifluoroacetic acid (400 mL). After stirring for 3 hours, the solvents were evaporated in vacuo and the thick oily residue was dissolved in diethyl ether (1.5 L) and refrigerated (72 hours). The white precipitate was filtered, washed with diethyl ether (300 mL) and dried to yield 59.4 g (85%) of white powder.

出典