Diethyl Ether → Methyl 4-(1,2,4-triazol-1-yl)-2-trifluoromethylbenzoate

HRID 1004418ノート

反応式

HRID 1004418 の反応式
F[C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([C:12]([F:15])([F:14])[F:13])[CH:3]=1.[NH:16]1[CH:20]=[N:19][CH:18]=[N:17]1.C(=O)([O-])[O-].[K+].[K+].CCOCC>CN(C)C=O>[N:16]1([C:2]2[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([C:12]([F:15])([F:14])[F:13])[CH:3]=2)[CH:20]=[N:19][CH:18]=[N:17]1

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 15541084Methyl 4-fluoro-2-(trifluoromethyl)benzoate

生成物 1

HCID 18795041Methyl 4-(1,2,4-triazol-1-yl)-2-trifluoromethylbenzoate収率 83.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

To a solution of methyl 4-fluoro-2-trifluoromethylbenzoate (4.95 g) in N,N-dimethylformamide was added 1,2,4-triazole (2.0 g) and potassium carbonate (4.0 g) at 20° C. and the mixture stirred for 4 hours at 60° C. The mixture was diluted (ether), washed (aqueous citric acid) and dried (magnesium sulfate). The residue was purified by chromatography to give methyl 4-(1,2,4-triazol-1-yl)-2-trifluoromethylbenzoate (5.07 g), NMR 3.98(s,3H),7.94-8.05(2H),8.15(2H),8.71(s,1H).

後処理

  1. washwashed (aqueous citric acid)
  2. dry with materialdried (magnesium sulfate)
  3. customThe residue was purified by chromatography

出典と根拠

ORDレコード
ord-5c285fe04e074a14ab30e015a3502f8e
出典データセット
uspto-grants-2000_04
特許番号
US06048984

反応ノート

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