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

HRID 477778
ノート
印刷プレビュー

反応式

HRID 477778 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-cb5d18deb64a41ddb87a83b3376adff0
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04889858

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート