Thionyl Chloride → 2-Chlorocarbonyl-6,11-dihydro-11-oxodibenz[b,e]oxepin

HRID 894192ノート

反応式

HRID 894192 の反応式
[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]([OH:19])=O)=[CH:16][C:3]1=2.S(Cl)([Cl:22])=O>>[Cl:22][C:17]([C:15]1[CH:14]=[CH:13][C:4]2[O:5][CH2:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[C:2](=[O:1])[C:3]=2[CH:16]=1)=[O:19]

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 12446821Olopatadine Impurity 17

生成物 1

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

実験手順

Heat a solution of 5 gm. of 6,11-dihydro-11-oxodibenz[b,e]oxepin-2-carboxylic acid and 40 ml. of thionyl chloride under reflux for 20 minutes. Evaporate the reaction mixture under vacuum to dryness. Repeat the evaporation with two 30 ml. portions of carbon tetrachloride. Crystallize the residue from diisopropyl ether to obtain the title product.

後処理

  1. temperatureHeat a solution of 5 gm
  2. customEvaporate the reaction mixture under vacuum to dryness
  3. customRepeat the evaporation with two 30 ml
  4. customCrystallize the residue from diisopropyl ether

出典と根拠

ORDレコード
ord-03917c48796442249d1cb806af3c04d1
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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