反応 #1994225

反応方程式

HCl

Rotigotine HCl

Boc-Glycine-OH

DCC

→

Boc-Gly Rotigotine

溶媒

diethyl ether

dichloromethane

反応条件

後処理

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

実験手順

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).

出典