반응 #49210

반응 방정식

Compound 94

1-{2-[Bis-(4-methoxy-phenyl)-phenyl-methoxymethyl}-4-hydroxy-pyrrolidin-1-yl]-6-dimethylamino-hexan-1-one

succinic anhydride

triethylamine

→

compound 96

Succinic acid mono-[5-[bis-(4-methoxy-phenyl)-phenyl-methoxymethyl]-1-(6-dimethylamino-hexanoyl)-pyrrolidin-3-yl]ester

용매

dichloromethane

반응 조건

후처리

1. 1
   기타dried in a vacuum at 40° C. overnight
2. 2
   workup.DISSOLUTIONThe mixture is dissolved in anhydrous dichloromethane (5 mL)
3. 3
   세척washed with ice cold aqueous citric acid (5% wt., 100 mL) and water (2×100 mL)
4. 4
   건조The organic phase is dried over anhydrous sodium sulfate
5. 5
   농축concentrated to dryness
6. 6
   기타The crude product is purified by column chromatography

실험 절차

Referring to scheme 25, Compound 94 (1.2 g, 2 mmol) is mixed with succinic anhydride (0.200 g, 2 mmol) and DMAP (0.244 g, 13 mmol) and dried in a vacuum at 40° C. overnight. The mixture is dissolved in anhydrous dichloromethane (5 mL), triethylamine (0.476 g, 0.64 mL, 4 mmol) is added and the solution stirred at room temperature under argon atmosphere for 16 h. It is then diluted with dichloromethane (100 mL) and washed with ice cold aqueous citric acid (5% wt., 100 mL) and water (2×100 mL). The organic phase is dried over anhydrous sodium sulfate and concentrated to dryness. The crude product is purified by column chromatography to afford compound 96.

출처