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Acetonitrile → 3,3-Bis-fluoromethyl-1-(4-chlorophenoxy)-1-(1,2,4-triazol-4-yl)-butan-2-one

HRID 851130
ノート
印刷プレビュー

反応式

HRID 851130 の反応式
[F:1][CH2:2][C:3]([CH2:17][F:18])([CH3:16])[C:4](=[O:15])[CH:5](Br)[O:6][C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1.N1C=[CH:22][N:21]=[N:20]1.[C:24](#[N:26])C>C(Cl)Cl>[F:1][CH2:2][C:3]([CH2:17][F:18])([CH3:16])[C:4](=[O:15])[CH:5]([O:6][C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)[N:26]1[CH:22]=[N:21][N:20]=[CH:24]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6342AcetonitrileHCID 130194363,3-Bis-fluoromethyl-1-bromo-1-(4-chlorophenoxy)-butan-2-oneHCID 178418936HCID 178418936、化合物

生成物 1

HCID 571626153,3-Bis-fluoromethyl-1-(4-chlorophenoxy)-1-(1,2,4-triazol-4-yl)-butan-2-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
50 °C

実験手順

82 g (0.286 mol) of 3,3-bis-fluoromethyl-1-bromo-1-(4-chlorophenoxy)-butan-2-one and 41.5 g (0.588 mol) of triazole were introduced into 600 ml of acetonitrile, the mixture was heated at 50° C. for 5 hours, the solvent was driven off under a waterpump vacuum, the residue was taken up in one liter of methylene chloride, the methylene chloride mixture was washed twice with 1,000 ml of water each time, the organic phase was dried over sodium sulphate and the solvent was distilled off. The residue was taken up in 500 ml of diisopropyl ether and the precipitate was filtered off. 6 g of 3,3-bis-fluoromethyl-1-(4-chlorophenoxy)-1-(1,2,4-triazol-4-yl)-butan-2-one (compound 3) of melting point 119°-122° C. were obtained. The mother liquor was distilled. 32.1 g (40% of theory) of 3,3-bis-fluoromethyl-1-(4-chlorophenoxy)-1-(1,2,4-triazol-1-yl)-butan-2-one (compound 4) of boiling point 160° -166° C./0.2 mm Hg were obtained.

後処理

  1. washthe methylene chloride mixture was washed twice with 1,000 ml of water each time
  2. dry with materialthe organic phase was dried over sodium sulphate
  3. distillationthe solvent was distilled off
  4. filtrationthe precipitate was filtered off

出典と根拠

ORDレコード
ord-f91518ddb2ce44d8afca79ceb6fe5f46
出典データセット
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04382944

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート