1,2-Dibromoethane → HCID 13650453、化合物

HRID 2290751ノート

反応式

HRID 2290751 の反応式
[N:1]1([CH2:6][C:7]([C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=2)=[O:8])[CH:5]=[N:4][CH:3]=[N:2]1.[CH2:16]1OCCOCCOCCOCCOCCO[CH2:17]1.[OH-].[K+].BrCCBr>C(Cl)Cl>[F:15][C:12]1[CH:13]=[CH:14][C:9]([C:7]([C:6]2([N:1]3[CH:5]=[N:4][CH:3]=[N:2]3)[CH2:17][CH2:16]2)=[O:8])=[CH:10][CH:11]=1

参加物

6

反応物 4

HCID 78391,2-DibromoethaneHCID 14797Potassium HydroxideHCID 2855718-Crown-6HCID 104204761-(4-Fluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethanone

生成物 1

HCID 13650453HCID 13650453、化合物収率 25%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(1H-1,2,4-triazol-1-yl)-4'-fluoroacetophenone (10.24 g, 50 mMole) in methylene chloride (70 ml) was added 18-Crown-6 ether (1 g) (trade mark for 1,4,7,10,13,16-hexaoxacyclooctadecane) and potassium hydroxide (6.1 g, 109 mMole) with stirring. Ten minutes later 1,2-dibromoethane was added (10.3 g, 55 mMole in one batch. Stirring was continued for 18 hours. The mixture was poured into saturated saline solution (100 ml) and the organic phase was separated, washed with water (3×30 ml) and dried over anhydrous magnesium sulphate. Evaporation gave an oil, weight 13.7 g. Purification was carried out by flash column chromatography under slight pressure (2 p.s.i.) on a Merck "Kieselgel 60" (trade mark) 230-400 mesh fractions after collection and evaporation gave a solid, the pure title compound, 2.9 g, m.p. 73°-75° (25% yield).

後処理

  1. stirringStirring
  2. customthe organic phase was separated
  3. washwashed with water (3×30 ml)
  4. dry with materialdried over anhydrous magnesium sulphate
  5. customEvaporation
  6. customgave an oil, weight 13.7 g
  7. customPurification
  8. customafter collection and evaporation
  9. customgave a solid

出典と根拠

ORDレコード
ord-08f38186bbaf4be58f8aa29e8a73f655
出典データセット
uspto-grants-1986_10
特許番号
US04618616

反応ノート

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