Triadimefon → Triadimenol

HRID 1758080

反応式

HRID 1758080 の反応式
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][CH:7]([N:14]2[CH:18]=[N:17][CH:16]=[N:15]2)[C:8](=[O:13])[C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:4][CH:3]=1.C(O)=O.C(N(CC)CC)C>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH:7]([N:14]2[CH:18]=[N:17][CH:16]=[N:15]2)[CH:8]([OH:13])[C:9]([CH3:11])([CH3:12])[CH3:10])=[CH:19][CH:20]=1

参加物

3

反応物 2

HCID 39385TriadimefonHCID 11084032Triethylammonium formate

生成物 1

HCID 41368Triadimenol収率 63.6%

実験手順

28.45 g (0.1 mol) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one and 43.25 g (0.1 mol) of formic acid/triethylamine (5:2 addition compound) were heated to 145° to 150° C. for 4.5 to 5 hours. The reaction mixture was allowed to cool and was concentrated in vacuo. The residue was taken up in dilute sodium hydroxide solution and the mixture was extracted with methylene chloride. The organic phase was washed with water, dried over sodium sulphate and concentrated in vacuo. The residue was suspended in hot cyclohexane, the suspension was filtered hot and the solid was dried. 18.2 g (63.6% of theory) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol of melting point 114°-116° C. were obtained.

後処理

  1. temperatureto cool
  2. concentrationwas concentrated in vacuo
  3. extractionthe mixture was extracted with methylene chloride
  4. washThe organic phase was washed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo
  7. filtrationthe suspension was filtered hot
  8. customthe solid was dried

出典と根拠

ORDレコード
ord-85245272f8394fb79a7fafd46c69355d
出典データセット
uspto-grants-1983_02
特許番号
US04371700

関連ノート

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