반응 #53624

반응 방정식

Magnesium

compound ( 55 )

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

→

titled compound

수율 79.0%

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

수율 79.0%

용매

chloroform

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONIce was added to the reaction mixture which
2. 2
   여과The insoluble materials were filtered off through cerite and the filtrate
3. 3
   추출was extracted with chloroform
4. 4
   세척The extracts were washed with brine
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   농축concentrated under reduced pressure
7. 7
   기타The residue obtained
8. 8
   기타was chromatographed on aluminum oxide in chloroform:hexane (2:1)

실험 절차

Magnesium (turning) 246 mg was added to compound (55) in methanol 9 ml and the mixture was stirred at room temperature for 3 h. Ice was added to the reaction mixture which was diluted with chloroform. The insoluble materials were filtered off through cerite and the filtrate was extracted with chloroform. The extracts were washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was chromatographed on aluminum oxide in chloroform:hexane (2:1) to give the titled compound as a pale yellow oil 97.8 mg. Yield 79%. This was treated with 1 eq. oxalic acid to give the salt, which was recrystallized from ether-methanol to give colorless crystals, m.p. 236-237° C. (dec.).

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