반응 #1683

반응 방정식

trifluoroacetic acid

Boc-D-Phe-Pro-OBn

anisole

→

white powder

수율 85.0%

D-Phe-Pro-OBn.TFA

수율 85.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   기타the solvents were evaporated in vacuo
2. 2
   workup.DISSOLUTIONthe thick oily residue was dissolved in diethyl ether (1.5 L)
3. 3
   기타(72 hours)
4. 4
   여과The white precipitate was filtered
5. 5
   세척washed with diethyl ether (300 mL)
6. 6
   기타dried

실험 절차

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.

출처