反応 #1851982

反応方程式

ethyl (6bR,10aS)-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate

KOH

→

title compound

収率 87.7%

(6bR,10aS)-2,3,6b,7,8,9,10,10a-octahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline

収率 87.7%

溶媒

n-butanol

反応条件

後処理

1. 1
   その他The solvent was removed under reduced pressure
2. 2
   workup.ADDITIONTo the residue was added water (30 mL)
3. 3
   抽出extracted with CH2Cl2 (3×50 mL)
4. 4
   洗浄The combined organic layers were washed with brine
5. 5
   乾燥dried over MgSO4
6. 6
   濃縮concentrated

実験手順

To ethyl (6bR,10aS)-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (4.10 g, 14.3 mmol) was added n-butanol (18.0 mL) and KOH powder (3.0 g). The reaction was heated at 199° C. in a sealed tube for 18 hr. The solvent was removed under reduced pressure. To the residue was added water (30 mL) extracted with CH2Cl2 (3×50 mL). The combined organic layers were washed with brine, dried over MgSO4, and concentrated to afford the title compound as a pale yellow oil (2.70 g, 78%). MS-ESI: 216 [MH]+

出典