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

HRID 894193노트

반응식

HRID 894193 반응식
Cl[C:2]([C:4]1[CH:19]=[CH:18][C:7]2[O:8][CH2:9][C:10]3[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=3[C:12](=[O:13])[C:6]=2[CH:5]=1)=[O:3].[NH3:20]>O1CCCC1>[O:13]=[C:12]1[C:11]2[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=2[CH2:9][O:8][C:7]2[CH:18]=[CH:19][C:4]([C:2]([NH2:20])=[O:3])=[CH:5][C:6]1=2

참가 물질

4

반응물 2

HCID 222Ammonia2회HCID 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 8028Tetrahydrofuran용매2회

실험 절차

Dissolve the acid chloride from Step A in 20 ml. of dry tetrahydrofuran and add this solution dropwise with stirring to a cooled (ice-bath) saturated solution of ammonia in 60 ml. of tetrahydrofuran. Pass ammonia through the reaction mixture simultaneously for 15 minutes. Stir at room temperature for an additional 15 minutes and evaporate the reaction mixture to dryness. Add a mixture of 12 ml. of ethanol and 60 ml. of water to the residue and stir at room temperature for an additional 30 minutes. Separate the solid by filtration and wash with water, then with ethanol and then with ether. Dry in vacuo to obtain the title product.

후처리

  1. stirringStir at room temperature for an additional 15 minutes
  2. customevaporate the reaction mixture to dryness
  3. additionAdd
  4. additiona mixture of 12 ml
  5. stirringof water to the residue and stir at room temperature for an additional 30 minutes
  6. customSeparate the solid
  7. filtrationby filtration
  8. washwash with water
  9. customDry in vacuo

출처 및 근거

ORD 기록
ord-273c4663703e4349988802136b904ff6
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282365

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