반응 #1994225

반응 방정식

HCl

Rotigotine HCl

Boc-Glycine-OH

DCC

→

Boc-Gly Rotigotine

용매

diethyl ether

dichloromethane

반응 조건

후처리

1. 1
   기타to give a suspension
2. 2
   여과The mixture was filtered
3. 3
   여과using filter paper
4. 4
   기타The layers were separated
5. 5
   추출the aqueous phase was extracted with 7 mL of dichloromethane
6. 6
   세척The combined organic phases were washed with water
7. 7
   건조with brine, dried over Na2SO4
8. 8
   여과filtered
9. 9
   농축concentrated
10. 10
    기타a rotary evaporator
11. 11
    기타dried in vacuo
12. 12
    기타to give a crude pale yellow solid
13. 13
    여과filtered on a glass frit
14. 14
    세척washed with diethyl ether
15. 15
    기타dried in vacuo

실험 절차

Rotigotine HCl (1.2 g, 3.41 mmol) and Boc-Glycine-OH (1.195 g, 6.82 mmol) were dissolved in dichloromethane (150 ml) to give a suspension. After addition of DMAP (0.625 g, 5.11 mmol) and DCC (1.407 g, 6.82 mmol), the mixture was stirred for 16 hours at room temperature. The mixture was filtered using filter paper and the filtrate was quenched with 51 mL of 0.1 N HCl (5.11 mmol). The layers were separated and the aqueous phase was extracted with 7 mL of dichloromethane. The combined organic phases were washed with water and then with brine, dried over Na2SO4, filtered, concentrated using a rotary evaporator, and dried in vacuo to give a crude pale yellow solid. The crude material was stirred with diethyl ether (50 mL) for 30 minutes, filtered on a glass frit, washed with diethyl ether, and dried in vacuo to give a pale yellow powder Boc-Gly-Rotigotine.HCl (1.258 g, 75% yield).

출처