Water → (5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazole-4-yl)-methanethiol

HRID 854126ノート

反応式

HRID 854126 の反応式
Br.[F:2][CH:3]([F:20])[O:4][C:5]1[N:9]([CH3:10])[N:8]=[C:7]([C:11]([F:14])([F:13])[F:12])[C:6]=1[CH2:15][S:16]C(=N)N.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[F:20][CH:3]([F:2])[O:4][C:5]1[N:9]([CH3:10])[N:8]=[C:7]([C:11]([F:14])([F:13])[F:12])[C:6]=1[CH2:15][SH:16]

参加物

5

反応物 3

HCID 962Water2 回HCID 11430Potassium CarbonateHCID 230756895-(Difluoromethoxy)-1-methyl-3-(trifluoromethyl)-1H-pyrazol-4-yl-carbamimidothioic acid methyl ester hydrobromide

生成物 1

HCID 23075696(5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazole-4-yl)-methanethiol収率 96.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1.00 g (2.60 mmol) of 2-(5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazole-4-ylmethyl)-isothiourea hydrobromide in 2 ml of N,N-dimethylformamide were added 0.43 g (3.12 mmol) of anhydrous potassium carbonate and 1 ml of water, followed by 1 hour of stirring at room temperature. After the completion of the reaction was confirmed, the reaction solution was poured into water and extracted with diethyl ether. The resulting organic layer was washed with water and then dried over anhydrous magnesium sulfate. The solvent was removed by evaporation under reduced pressure to obtain 0.66 g (purity: 84.9%, yield: 82.4%) of (5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazole-4-yl)-methanethiol.

後処理

  1. extractionextracted with diethyl ether
  2. washThe resulting organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-77a2252fd4974fef8747afef180688a1
出典データセット
uspto-grants-2007_08
特許番号
US07256298B2

反応ノート

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