Dimethylformamide → 5-methyl-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxylic acid chloride

HRID 1748610ノート

反応式

HRID 1748610 の反応式
[CH3:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][N:8]=2)[N:5]=[CH:4][C:3]=1[C:17]([OH:19])=O.CN(C)C=O.S(Cl)([Cl:27])=O>C1(C)C=CC=CC=1>[CH3:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][N:8]=2)[N:5]=[CH:4][C:3]=1[C:17]([Cl:27])=[O:19]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 162278455-methyl-1-(5-(trifluoromethyl)pyridin-2-yl)-1H-pyrazole-4-carboxylic acid

生成物 1

HCID 897349975-methyl-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxylic acid chloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

To a solution of 5-methyl-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxylic acid (40.0 g) described in Reference Example 8 in toluene (147 ml) were added N,N-dimethylformamide (catalyst quantity) and thionyl chloride (52.6 g) at room temperature, and stirred at 80° C. for 4.5 hours. After completion of the reaction, the solvent and excessive thionyl chloride were evaporated, azeotropy was performed with toluene twice, and then dried in vacuo to give the titled compound as a pale yellow solid.

後処理

  1. customAfter completion of the reaction
  2. customthe solvent and excessive thionyl chloride were evaporated
  3. customdried in vacuo

出典と根拠

ORDレコード
ord-5ee31dcb134e4a2ab06647809297759a
出典データセット
uspto-grants-2015_10
特許番号
US09150555B2

反応ノート

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