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1H-1,2,4-Triazole → HCID 13259987, 화합물

HRID 2166357
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HRID 2166357 반응식
[Na].[NH:2]1[CH:6]=[N:5][CH:4]=[N:3]1.[Cl:7][C:8]1[CH:9]=[C:10]([C:15]2([CH2:18][C:19]#[CH:20])[CH2:17][O:16]2)[CH:11]=[CH:12][C:13]=1[Cl:14]>C(O)CCC>[Cl:7][C:8]1[CH:9]=[C:10]([C:15]([OH:16])([CH2:17][N:2]2[CH:6]=[N:5][CH:4]=[N:3]2)[CH2:18][C:19]#[CH:20])[CH:11]=[CH:12][C:13]=1[Cl:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 92571H-1,2,4-TriazoleHCID 5360545SodiumHCID 132599842-(3,4-Dichlorophenyl)-2-(prop-2-yn-1-yl)oxirane

생성물 1

HCID 13259987HCID 13259987, 화합물수율 59.3%

시약·촉매·용매 1

HCID 2631-Butanol용매2회

실험 절차

0.275 g (0.011 mol) of sodium is introduced into a boiling solution of 8.05 g (0.116 mol) of 1,2,4-triazole in 400 ml of n-butanol. 24 g (0.105 mol) of 2-(3,4-dichlorophenyl)-2-propargyl-oxirane, dissolved in 50 ml of n-butanol, are then added. The solution is heated at the boil for 12 hours, the solvent is distilled off in vacuo, the residue is taken up in 200 ml of trichloromethane, the solution is washed with twice 50 ml of water, and the organic phase is dried over anhydrous sodium sulphate and then filtered over 200 g of silica gel. 18.45 g (53.6% of theory) of 4-(3,4-dichlorophenyl)-5-(1,2,4-triazol-1-yl)-pent-1-in-4-ol are obtained as colorless crystals of melting point 114° C.

후처리

  1. additionare then added
  2. temperatureThe solution is heated at the boil for 12 hours
  3. distillationthe solvent is distilled off in vacuo
  4. washthe solution is washed with twice 50 ml of water
  5. dry with materialthe organic phase is dried over anhydrous sodium sulphate
  6. filtrationfiltered over 200 g of silica gel

출처 및 근거

ORD 기록
ord-675775e353f246d581c4f88516f97d48
출처 데이터셋
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04945101

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