Methanol → Methyl 3-(chloromethyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylate

HRID 885786노트

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HRID 885786 반응식
[ClH:1].[Cl:2][C:3]1[C:4]([N:9]2[C:13]([C:14]([OH:16])=[O:15])=[CH:12][C:11]([CH2:17]O)=[N:10]2)=[N:5][CH:6]=[CH:7][CH:8]=1.O=S(Cl)Cl.[CH3:23]O>C1(C)C=CC=CC=1>[Cl:1][CH2:17][C:11]1[CH:12]=[C:13]([C:14]([O:16][CH3:23])=[O:15])[N:9]([C:4]2[C:3]([Cl:2])=[CH:8][CH:7]=[CH:6][N:5]=2)[N:10]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 666806641-(3-chloropyridin-2-yl)-3-(hydroxymethyl)-1H-pyrazole-5-carboxylic acid hydrochloride

생성물 1

HCID 49850068Methyl 3-(chloromethyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylate

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
70 °C

실험 절차

1-(3-chloropyridin-2-yl)-3-(hydroxymethyl)-1H-pyrazole-5-carboxylic acid hydrochloride (0.1 mol) was initially charged in 100 ml of toluene. 24 g of SOCl2 were added in portions at 60° C. The mixture was heated at 70° C. for 3 h, in the course of which the precipitate went completely into the solution. Methanol (30 ml) was slowly added dropwise to the mixture and the solution was stirred at 30° C. for a further 1 h. Subsequently, the solution was concentrated under reduced pressure. This gave 95% of the product with a purity of 96%.

후처리

  1. concentrationSubsequently, the solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9e39da07d8af494ab8d95c5a0dc46cd3
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242313B2

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