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Methyl chloroacetate → HCID 20475380, 화합물

HRID 443589
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HRID 443589 반응식
Cl[CH2:2][C:3]([O:5][CH3:6])=[O:4].[CH2:7]([NH:11][C:12](=S)[NH:13][NH2:14])[CH:8]([CH3:10])[CH3:9].O1CC[CH2:18][CH2:17]1>>[CH2:7]([NH:11][C:12]1[C:2]([C:3]([O:5][CH3:6])=[O:4])=[C:17]([CH3:18])[NH:14][N:13]=1)[CH:8]([CH3:10])[CH3:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 7295Methyl chloroacetateHCID 8028TetrahydrofuranHCID 12367441HCID 12367441, 화합물

생성물 1

HCID 20475380HCID 20475380, 화합물

실험 절차

15.1 g of methyl 2-chloroacetate is added to a suspension of 14.7 g of 4-isobutylthiosemicarbazide in 150 ml of tetrahydrofuran. The mixture is stirred for 30 minutes and then boiled. After stirring for a further hour at 65° C., the mixture is cooled, the precipitated solid is isolated and washed with acetone. The residue is dissolved hot in water, filtered off from the precipitated sulfur and, after cooling, aqueous ammonia solution is added. After suction filtering and drying the product, 3-isobutylamino-4-methoxycarbonyl-5-methylpyrazole is isolated; m.p. 100°-103° C.

후처리

  1. stirringAfter stirring for a further hour at 65° C.
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
temperature
the mixture is cooled
  • customthe precipitated solid is isolated
  • washwashed with acetone
  • dissolutionThe residue is dissolved hot in water
  • filtrationfiltered off from the precipitated sulfur
  • temperatureafter cooling
  • additionaqueous ammonia solution is added
  • filtrationAfter suction filtering
  • customdrying the product
  • 출처 및 근거

    ORD 기록
    ord-b57116b2ced749d1999161d3c95a656d
    출처 데이터셋
    uspto-grants-1981_04
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04260775

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