반응 #1972919

반응 방정식

lithium aluminum hydride

nitrile

10-chloro-3-cyano-6,12-dimethyl-1,2,3,4,5,6-hexahydro-2,6-methano-9H-pyrrolo-[3,2-h][3]benzazocine

ethyl acetate

sodium hydroxide

→

product

수율 18.0%

10-Chloro-6,12-dimethyl-1,2,3,4,5,6-hexahydro-2,6-methano-9H-pyrrolo[3,2-h][3]benzazocine

수율 18.0%

용매

tetrahydrofuran

water

water

반응 조건

후처리

1. 1
   온도The suspension was heated
2. 2
   온도at reflux for 2 hr
3. 3
   여과The suspension was filtered
4. 4
   농축the filtrate was concentrated
5. 5
   기타The residue was triturated with ether
6. 6
   기타the solid was recrystallized from methanol

실험 절차

The nitrile (6.41 g) was dissolved in 300 ml of tetrahydrofuran and, 4.06 g lithium aluminum hydride was added, with stirring. The suspension was heated at reflux for 2 hr and ethyl acetate, water, aqueous sodium hydroxide solution and water were added. The suspension was filtered and the filtrate was concentrated. The residue was triturated with ether and the solid was recrystallized from methanol to give 0.64 g (18%) of the product, mp 260°-263° C. (dec.).

출처