反应 #1994225

反应方程式

HCl

Rotigotine HCl

Boc-Glycine-OH

DCC

→

Boc-Gly Rotigotine

溶剂

diethyl ether

dichloromethane

反应条件

后处理

1. 1
   其他to give a suspension
2. 2
   过滤The mixture was filtered
3. 3
   过滤using filter paper
4. 4
   其他The layers were separated
5. 5
   萃取the aqueous phase was extracted with 7 mL of dichloromethane
6. 6
   洗涤The combined organic phases were washed with water
7. 7
   干燥with brine, dried over Na2SO4
8. 8
   过滤filtered
9. 9
   浓缩concentrated
10. 10
    其他a rotary evaporator
11. 11
    其他dried in vacuo
12. 12
    其他to give a crude pale yellow solid
13. 13
    过滤filtered on a glass frit
14. 14
    洗涤washed with diethyl ether
15. 15
    其他dried in vacuo

实验过程

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).

来源