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Ethanol → 3-Fluorodibenz[b,e]oxepin-11(6H)-one

HRID 477778
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HRID 477778 반응식
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.C(O)C.[F:18][C:19]1[CH:20]=[C:21]([O:25][CH2:26][C:27]2[CH:35]=[CH:34][CH:33]=[CH:32][C:28]=2[C:29]([OH:31])=O)[CH:22]=[CH:23][CH:24]=1>O>[F:18][C:19]1[CH:24]=[CH:23][C:22]2[C:29](=[O:31])[C:28]3[CH:32]=[CH:33][CH:34]=[CH:35][C:27]=3[CH2:26][O:25][C:21]=2[CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 14812Phosphorus oxide (P4O10)HCID 117914642-[(3-fluorophenoxy)methyl]benzoic Acid

생성물 1

HCID 110751573-Fluorodibenz[b,e]oxepin-11(6H)-one수율 79.6%

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

To 250 g of phosphorus pentoxide is slowly added 160 ml of ethanol at room temperature. The mixture is further stirred with heating at 100° C. for 1 hour. Thereto 42 g of 2-[(3-fluorophenyloxy)methyl]benzoic acid is added and the mixture is stirred with heating at 100° C. for 1 hour. After cooling to room temperature, 500 ml of water is added. After extraction with toluene, washing successively with saturated sodium hydrogen carbonate, water and a saturated saline solution and drying over magnesium sulfate, the solvent is distilled off under reduced pressure to give 31 g of 3-fluoro-6,11-dihydrodibenz[b,e]oxepin-11-one (oil). Mass spectrum m/z: 228(M+).

후처리

  1. customat room temperature
  2. stirringthe mixture is stirred
  3. temperaturewith heating at 100° C. for 1 hour
  4. temperatureAfter cooling to room temperature
  5. extractionAfter extraction with toluene
  6. washwashing successively with saturated sodium hydrogen carbonate, water
  7. dry with materiala saturated saline solution and drying over magnesium sulfate
  8. distillationthe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-cb5d18deb64a41ddb87a83b3376adff0
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04889858

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