1H-1,2,4-Triazole → Tebuconazole

HRID 371487

반응식

HRID 371487 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]2([C:13]([CH3:16])([CH3:15])[CH3:14])[CH2:12][O:11]2)=[CH:4][CH:3]=1.[NH:17]1[CH:21]=[N:20][CH:19]=[N:18]1>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]([CH2:12][N:17]2[CH:21]=[N:20][CH:19]=[N:18]2)([OH:11])[C:13]([CH3:16])([CH3:15])[CH3:14])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 92571H-1,2,4-TriazoleHCID 946842-tert-Butyl-2-(2-(4-chlorophenyl)ethyl)oxirane

생성물 1

HCID 86102Tebuconazole수율 53.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyl-oxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol was heated in a bomb tube at 150° C. for 20 hours. The reaction solution was allowed to cool and was concentrated. The residue was dissolved in ether and the solution was washed three times with water and once with sodium chloride solution, dried over sodium sulphate and concentrated. The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-pentane-3-ol were obtained as a viscous oil.

후처리

  1. temperatureto cool
  2. concentrationwas concentrated
  3. dissolutionThe residue was dissolved in ether
  4. washthe solution was washed three times with water
  5. dry with materialonce with sodium chloride solution, dried over sodium sulphate
  6. concentrationconcentrated
  7. customThe residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1)

출처 및 근거

ORD 기록
ord-74db8e5bb66b41c095213b112c53683b
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04532341

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