Formaldehyde → methyl 1-(hydroxymethyl)-1H-pyrazole-4-carboxylate

HRID 1983025노트

반응식

HRID 1983025 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[N:7][NH:8][CH:9]=1)=[O:4].[CH2:10]=[O:11].C(N(CC)CC)C>CC(C)=O>[OH:11][CH2:10][N:7]1[CH:6]=[C:5]([C:3]([O:2][CH3:1])=[O:4])[CH:9]=[N:8]1

참가 물질

5

반응물 3

HCID 712Formaldehyde2회HCID 8471Triethylamine2회HCID 9793760Methyl 1H-pyrazole-4-carboxylate

생성물 1

HCID 23149172methyl 1-(hydroxymethyl)-1H-pyrazole-4-carboxylate수율 79.6%

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
130 °C

실험 절차

The mixture of 1.40 g of 4-methoxycarbonyl-1H-pyrazole, 0.37 g of paraformaldehyde and 0.11 g of triethylamine was stirred at 130° C. for 1 hour. 0.74 g of paraformaldehyde and 2 ml of triethylamine were added to the mixture and stirred at 130° C. for 2 hours. After the reaction mixture was cooled to room temperature, acetone was added. After the mixture was filtered, the filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 1.38 g of 1-(hydroxymethyl)-4-methoxycarbonyl-1H-pyrazole.

후처리

  1. stirringstirred at 130° C. for 2 hours
  2. temperatureAfter the reaction mixture was cooled to room temperature
  3. filtrationAfter the mixture was filtered
  4. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-33722893bd724639b992c6a8f08dda9d
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541374B2

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