반응 #2955

반응 방정식

(±)-trans-2-ethyl-4a-(3-methoxyphenyl)-6-oxo-1,2,3,4,4a,5,6,7,8,8a-decahydroisoquinoline hydrochloride

hydroxylamine hydrochloride

→

title compound

수율 96.6%

(±)-trans-2-Ethyl-6-hydroxyimino-4a-(3-methoxyphenyl)-1,2,3,4,4a,5,6,7,8, 8a-decahydroisoquinoline

수율 96.6%

용매

MeOH

반응 조건

후처리

1. 1
   여과The precipitate was filtered
2. 2
   기타the solvent was removed in vacuo
3. 3
   추출the aqueous layer was extracted with CH2Cl2
4. 4
   기타The organic layer was dried
5. 5
   기타the solvent removed in vacuo

실험 절차

0.5 g (1.54 mmol) of (±)-trans-2-ethyl-4a-(3-methoxyphenyl)-6-oxo-1,2,3,4,4a,5,6,7,8,8a-decahydroisoquinoline hydrochloride, 0.456 g (6.56 mmol) of hydroxylamine hydrochloride and 0.64 g of KHCO3 in 10 ml of MeOH were refluxed for 45 min. The precipitate was filtered, the solvent was removed in vacuo and the residue taken up in H2O. The pH was adjusted to 8 with conc. NH4OH, the aqueous layer was extracted with CH2Cl2. The organic layer was dried, the solvent removed in vacuo, obtaining 0.45 g of the title compound which was used as such in the subsequent step.

출처