反応 #53623

反応方程式

Compound ( 54 )

(2-Benzenesulfonyl-1-vinyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]azulen-8-yl)dimethylamine

→

titled compound

収率 98.4%

(2-Benzenesulfonyl-1-ethyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]azulen-8-yl)dimethylamine

収率 98.4%

溶媒

methanol

tetrahydrofuran

反応条件

後処理

1. 1
   ろ過The catalyst was filtered off
2. 2
   濃縮the filtrate was concentrated under reduced pressure
3. 3
   その他The residue obtained
4. 4
   その他was chromatographed on aluminum oxide in chloroform:hexane (1:1)

実験手順

Compound (54) 200.1 mg was dissolved in a mixture of methanol 8 ml and tetrahydrofuran 4 ml. 10% Pd/C 49.8 mg was added. The mixture was stirred under hydrogen atmosphere for 18 h at room temperature. The catalyst was filtered off and the filtrate was concentrated under reduced pressure. The residue obtained was chromatographed on aluminum oxide in chloroform:hexane (1:1) to give the titled compound as a colorless oil 198 mg. Yield 98%. This was treated with 1 eq. of oxalic acid to give the salt, which was recrystallized from ether-methanol to give colorless crystals, m.p. 193-194° C.(dec.).

出典