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Acetonitrile → HCID 54287444, 화합물

HRID 649517
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HRID 649517 반응식
Br[CH2:2][C:3]([C:13]([CH3:16])([CH3:15])[CH3:14])=[CH:4][C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=1[Cl:12].N1C=[CH:20][N:19]=[N:18]1.[C:22](#[N:24])C>>[Cl:12][C:6]1[CH:7]=[C:8]([Cl:11])[CH:9]=[CH:10][C:5]=1[CH:4]=[C:3]([CH2:2][N:19]1[CH:20]=[N:24][CH:22]=[N:18]1)[C:13]([CH3:16])([CH3:15])[CH3:14]
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참가 물질

4

반응물 3

HCID 6342AcetonitrileHCID 545259841-[2-(Bromomethyl)-3,3-dimethylbut-1-en-1-yl]-2,4-dichlorobenzeneHCID 178418936HCID 178418936, 화합물

생성물 1

HCID 54287444HCID 54287444, 화합물수율 24%

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온도
40 °C

실험 절차

A mixture of 20 g (0.062 mol) of 2-bromomethyl-1-(2,4-dichlorophenyl)-3,3-dimethylbut-1-ene and 8.6 g (0.125 mol) of triazole in 80 ml of absolute acetonitrile is stirred at 40° C. for 16 hours. For working up, the reaction mixture is filtered, the filtrate is concentrated in vacuo and the residue is taken up in methylene chloride. The mixture is washed twice with water, dried over sodium sulphate and concentrated in vacuo. The syrup which remains is purified by chromatography (silica gel) and crystallized from petroleum ether. 4.6 g (24% of theory) of 1-(2,4-dichlorophenyl)-3,3-dimethyl-2-(1,2,4-triazol-1-ylmethyl)-but-1-ene of melting point 78° C. are obtained.

후처리

  1. filtrationthe reaction mixture is filtered
  2. concentrationthe filtrate is concentrated in vacuo
  3. washThe mixture is washed twice with water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated in vacuo
  6. customThe syrup which remains is purified by chromatography (silica gel)
  7. customcrystallized from petroleum ether

출처 및 근거

ORD 기록
ord-15753be10dd54ef1ae95ae2497c66869
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04740515

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