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

HRID 633736노트

반응식

HRID 633736 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 31649321-methyl-1H-pyrazole-5-carbonyl chloride수율 97.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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:

후처리

  1. customevaporated to dryness
  2. customevaporated again

출처 및 근거

ORD 기록
ord-2c18608f5dbd48528357837ec0f99b15
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321790B2

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