Acetic Acid → 6,11-Dihydro-11-oxodibenz[b,e]oxepin-9-carboxylic Acid

HRID 894174노트

반응식

HRID 894174 반응식
[O:1]=[C:2]1[C:8]2[CH:9]=C(C#N)[CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:15]=[CH:16][CH:17]=[CH:18][C:3]1=2.[C:19]([OH:22])(=[O:21])[CH3:20].Cl>O>[O:1]=[C:2]1[C:8]2[CH:9]=[C:20]([C:19]([OH:22])=[O:21])[CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:15]=[CH:16][CH:17]=[CH:18][C:3]1=2

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 129291409-Cyano-6,11-dihydro-11-oxodibenz[b,e]oxepin

생성물 1

HCID 129291416,11-Dihydro-11-oxodibenz[b,e]oxepin-9-carboxylic Acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Reflux a mixture of 7.43 gm. (0.0316 mole) of 6,11-dihydro-11-oxodibenz[b,e]oxepin-9-carbonitrile, 130 ml. of acetic acid, 13 ml. of water and 13 ml. of concentrated hydrochloric acid for 156 hours. Cool the reaction mixture, separate the solids by filtration and dry (yield 6.20 gm., m.p. 264°-269° C.). Recrystallize from acetic acid to obtain the title product (m.p. 270.5°-271.5° C.).

후처리

  1. temperatureReflux
  2. additiona mixture of 7.43 gm
  3. temperatureCool the reaction mixture
  4. customseparate the solids
  5. filtrationby filtration
  6. customdry (yield 6.20 gm., m.p. 264°-269° C.)
  7. customRecrystallize from acetic acid

출처 및 근거

ORD 기록
ord-3d948dc3ebf44f6d8e59ec81c74c1bf0
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282365

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