반응 #2000564

반응 방정식

5′-(5-cyano-1-methyl-1H-pyrrol-2-yl)spiro[cyclohexane-1,3′-[3H]indol]-2′-ylidenecyanamide

diethylamine

→

5′-(5-cyano-1-methyl-1H-pyrrol-2-yl)spiro[cyclohexane-1,3′-[3H]indol]

수율 69.5%

용매

THF

THF

반응 조건

후처리

1. 1
   workup.DISSOLUTIONuntil dissolved
2. 2
   workup.DISTILLATIONThe solvent was distilled off (2.5 L) during which a precipitate
3. 3
   기타was formed
4. 4
   여과the white precipitate was filtered
5. 5
   세척washed with ether
6. 6
   기타dried

실험 절차

Crude 5′-(5-cyano-1-methyl-1H-pyrrol-2-yl)spiro[cyclohexane-1,3′-[3H]indol]-2′-ylidenecyanamide (95.0 g; purity 78% HPLC area) in THF (250 mL) was treated with diethylamine (105 g) and refluxed with a concomitant addition of THF (3.35 L) until dissolved. The solvent was distilled off (2.5 L) during which a precipitate was formed. The flask was cooled to ambient temperature and the white precipitate was filtered, washed with ether and dried to give 58.0 g (61% yield) of purified 5′-(5-cyano-1-methyl-1H-pyrrol-2-yl)spiro[cyclohexane-1,3′-[3H]indol])-2′-ylidenecyanamide (purity>99% HPLC area).

출처