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

HRID 894174ノート

反応式

HRID 894174 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-3d948dc3ebf44f6d8e59ec81c74c1bf0
出典データセット
uspto-grants-1981_08
特許番号
US04282365

反応ノート

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