反応 #2955

反応方程式

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

hydroxylamine hydrochloride

→

title compound

収率 96.6%

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

収率 96.6%

溶媒

MeOH

反応条件

後処理

1. 1
   ろ過The precipitate was filtered
2. 2
   その他the solvent was removed in vacuo
3. 3
   抽出the aqueous layer was extracted with CH2Cl2
4. 4
   その他The organic layer was dried
5. 5
   その他the solvent removed in vacuo

実験手順

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.

出典