Acetic Acid → 6,11-Dihydro-11-ethylidenedibenz[b,e]oxepin-2-carboxylic Acid

HRID 894222ノート

反応式

HRID 894222 の反応式
C(C1[CH:19]=[CH:18][C:6]2[O:7][CH2:8][C:9]3[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=3[C:11](=[CH:12][CH3:13])[C:5]=2[CH:4]=1)#N.[C:20]([OH:23])(=[O:22])[CH3:21].Cl>O>[CH:12](=[C:11]1[C:10]2[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=2[CH2:8][O:7][C:6]2[CH:18]=[CH:19][C:21]([C:20]([OH:23])=[O:22])=[CH:4][C:5]1=2)[CH3:13]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 536734252-Cyano-6,11-dihydro-11-ethylidenedibenz[b,e]oxepin

生成物 1

HCID 545396956,11-Dihydro-11-ethylidenedibenz[b,e]oxepin-2-carboxylic Acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Reflux a mixture of 2.8 gm of the nitrile of Step A, 50 ml of acetic acid, 5 ml of water and 5 ml of concentrated hydrochloric acid for 140 hours. Cool the reaction mixture, separate the solids by filtration and dry. Recrystallize from toluene to obtain the title product.

後処理

  1. temperatureReflux
  2. temperatureCool the reaction mixture
  3. customseparate the solids
  4. filtrationby filtration
  5. customdry
  6. customRecrystallize from toluene

出典と根拠

ORDレコード
ord-e65d07c7de3d4a0dbf28170e3b422d46
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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