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Benzoyl chloride → HCID 20187548、化合物

HRID 2308738
ノート
印刷プレビュー

反応式

HRID 2308738 の反応式
[C:1](Cl)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].[Cl:12][C:13]1[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:14]=1[CH:20](O)[CH:21]([F:27])[N:22]1[CH:26]=[N:25][CH:24]=[N:23]1>C(OCC)C>[Cl:12][C:13]1[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:14]=1[CH:20]([C:1](=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH:21]([F:27])[N:22]1[CH:26]=[N:25][CH:24]=[N:23]1
参加物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 7412Benzoyl chlorideHCID 14798Sodium HydroxideHCID 20187544HCID 20187544、化合物

生成物 1

HCID 20187548HCID 20187548、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

With efficient stirring, a solution of 25 ml of benzoyl chloride in 250 ml of diethyl ether is added dropwise at 0°-5° C. to a mixture of 250 ml of 2n NaOH solution and 27.6 g of 1-(2,4-dichlorophenyl)-2-fluoro-2-(1H-1,2,4-triazol-1-yl)ethanol (prepared in accordance with Example P1a). The reaction mixture is stirred for another 2 hours at 0°-5° C. and then further without cooling until it has reached room temperature. The separated ethereal phase is washed with four 50 ml portions of 0.2n NaOH solution and then with water until neutral, dried over sodium sulfate, filtered and concentrated by evaporation, affording as crude product 40 g of an oil which is purified by flash distillation at 0.07 mbar and 180° C. Recrystallisation from diisopropyl ether affords approx. 26 g of the product which melts at 104°-108° C.

後処理

  1. temperaturefurther without cooling until it
  2. customhas reached room temperature
  3. washThe separated ethereal phase is washed with four 50 ml portions of 0.2n NaOH solution
  4. dry with materialwith water until neutral, dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation
  7. customaffording as crude product 40 g of an oil which
  8. distillationis purified by flash distillation at 0.07 mbar and 180° C
  9. customRecrystallisation from diisopropyl ether

出典と根拠

ORDレコード
ord-20d6e54dd4154e1f863f352f57ff8c90
出典データセット
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04690942

反応ノート

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