1H-1,2,4-Triazole → Tebuconazole

HRID 979451

反応式

HRID 979451 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 86102Tebuconazole収率 53.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyloxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol in a sealed tube is heated at 150° C. for 20 hours. The tube is allowed to cool and the reaction solution is evaporated. The residue is dissolved in ether, washed three times with water and once with sodium chloride solution, dried over sodium sulphate and evaporated. The residue is chromatographed over a column of silican gel (mobile phase: dichloroethane/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)-3-pentanol are obtained as a viscous oil.

後処理

  1. temperatureto cool
  2. customthe reaction solution is evaporated
  3. dissolutionThe residue is dissolved in ether
  4. washwashed three times with water
  5. dry with materialonce with sodium chloride solution, dried over sodium sulphate
  6. customevaporated
  7. customThe residue is chromatographed over a column of silican gel (mobile phase: dichloroethane/ethyl acetate 1:1)

出典と根拠

ORDレコード
ord-7450237c8f7f43f99617dae5adba092e
出典データセット
uspto-grants-1987_05
特許番号
US04668660

関連ノート

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