1,2-Dibromoethane → HCID 13650453, 화합물

HRID 2290751노트

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HRID 2290751 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 13650453HCID 13650453, 화합물수율 25%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-08f38186bbaf4be58f8aa29e8a73f655
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04618616

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