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

HRID 894192노트

반응식

HRID 894192 반응식
[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]

참가 물질

3

반응물 2

HCID 24386Thionyl ChlorideHCID 12446821Olopatadine Impurity 17

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-03917c48796442249d1cb806af3c04d1
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282365

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