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Ammonia → 6,11-Dihydro-11-oxodibenz[b,e]oxepin-2-carboamide

HRID 1982372
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반응식

HRID 1982372 반응식
[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17](Cl)=[O:18])=[CH:16][C:3]1=2.[NH3:20]>O1CCCC1>[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([NH2:20])=[O:18])=[CH:16][C:3]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 134560052-Chlorocarbonyl-6,11-dihydro-11-oxodibenz[b,e]oxepin

생성물 1

HCID 124468236,11-Dihydro-11-oxodibenz[b,e]oxepin-2-carboamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The remaining half of the acid chloride IV was added to a mixture of 150 ml of concentrated ammonia and 150 ml of tetrahydrofuran. Then, the mixture was stirred at room temperature for three hours and concentrated under reduced pressure. The residue was vigorously stirred together with 300 ml of saturated aqueous solution of sodium bicarbonate and 100 ml of ether, and the solid was collected by filtration and dried to obtain 6,11-dihydro-11-oxodibenz[b,e]oxepin-2-carboamide VIII in a quantitative yield. Recrystallization from methanol gave pure crystals having a melting point of 227°-228° C. IR spectrum (KBr tablet, cm-1): 3430, 3150, 1680, 1635, 1600, 1370.

후처리

  1. concentrationconcentrated under reduced pressure
  2. stirringThe residue was vigorously stirred together with 300 ml of saturated aqueous solution of sodium bicarbonate and 100 ml of ether
  3. filtrationthe solid was collected by filtration
  4. customdried

출처 및 근거

ORD 기록
ord-964c45345b2b4a7296b2a45afb0ef1fa
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04596804

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