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Thionyl Chloride → 5-Methyl-4-imidazolecarbonyl chloride hydrochloride

HRID 1719257
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HRID 1719257 반응식
[ClH:1].[CH3:2][C:3]1[NH:7][CH:6]=[N:5][C:4]=1[C:8]([OH:10])=O.S(Cl)([Cl:13])=O>CN(C)C=O.C1(C)C=CC=CC=1>[ClH:13].[CH3:2][C:3]1[NH:7][CH:6]=[N:5][C:4]=1[C:8]([Cl:1])=[O:10]
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참가 물질

5

반응물 2

HCID 24386Thionyl ChlorideHCID 131606155-Methyl-1H-imidazole-4-carboxylic acid hydrochloride (1:1)

생성물 1

HCID 202680275-Methyl-4-imidazolecarbonyl chloride hydrochloride수율 70.1%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

To a suspension of 880 g (5.4 moles) of 5-methyl-4-imidazolecarboxylic acid hydrochloride in 100 ml of dimethylformamide and 2 liters of toluene at 60° C., there was added slowly over 2 hours 790 ml (10.8 moles) of thionyl chloride. At the end of the addition, the mixture was held with good stirring for 1 hour at 80° C. It was allowed to cool, filtered, the solid was washed with 1 liter of toluene. 685 g of 5-methyl-4-imidazolecarbonyl chloride hydrochloride were obtained.

후처리

  1. additionAt the end of the addition
  2. temperatureto cool
  3. filtrationfiltered
  4. washthe solid was washed with 1 liter of toluene

출처 및 근거

ORD 기록
ord-1508279536a140268bb6e1de6bc96243
출처 데이터셋
uspto-grants-1985_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04539331

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