Dimethylformamide → 1-methyl-1H-pyrazole-5-carbonyl chloride

HRID 633736ノート

反応式

HRID 633736 の反応式
[CH3:1][N:2]1[C:6]([C:7]([OH:9])=O)=[CH:5][CH:4]=[N:3]1.C(Cl)(=O)C([Cl:13])=O.CN(C=O)C>C(Cl)Cl>[CH3:1][N:2]1[C:6]([C:7]([Cl:13])=[O:9])=[CH:5][CH:4]=[N:3]1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 6431581-methyl-1H-pyrazole-5-carboxylic acid

生成物 1

HCID 31649321-methyl-1H-pyrazole-5-carbonyl chloride収率 97.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

A suspension of 800 mg (6.03 mmol) of 2-methyl-2H-pyrazole-3-carboxylic acid in 30 mL of DCM is placed under argon and cooled to 0° C. When the temperature is reached, 1.32 mL (15.07 mmol) of oxalyl chloride and a catalytic amount of DMF are added. The reaction mixture is stirred at room temperature for 2 hours and then evaporated to dryness and the residue is taken up in DCM and evaporated again to give 850 mg of 2-methyl-2H-pyrazole-3-carbonyl chloride, the characteristics of which are as follows:

後処理

  1. customevaporated to dryness
  2. customevaporated again

出典と根拠

ORDレコード
ord-2c18608f5dbd48528357837ec0f99b15
出典データセット
uspto-grants-2016_04
特許番号
US09321790B2

反応ノート

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