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Methylhydrazine → HCID 178488709, 화합물

HRID 628532
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HRID 628532 반응식
C([O:3][C:4](=O)[CH2:5][C:6]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([CH3:16])[CH:9]=1)=O)C.[CH3:18][NH:19][NH2:20]>C1(C)C=CC=CC=1>[OH:3][C:4]1[N:19]([CH3:18])[N:20]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([CH3:16])[CH:9]=2)[CH:5]=1
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참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 21243218Ethyl 3-(4-methoxy-3-methylphenyl)-3-oxopropanoate

생성물 1

HCID 178488709HCID 178488709, 화합물수율 68%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

At room temperature, to a mixture of 3-(4-methoxy-3-methyl-phenyl)-3-oxo-propionic acid ethyl ester (described in Reference Preparation example 89) 14.8 g and toluene 100 ml was added N-methyl hydrazine 29 g, and the resulting mixture was stirred for twelve hours. The toluene was distilled off. At room temperature, to the reaction mixture was added water 100 ml and the resulting mixture was acidified with 10% aqueous hydrochloric acid solution and was stirred for three hours. The precipitates were filtered and were washed with water 400 ml and ethyl acetate 500 ml, and then were dried under reduced pressure to give 5-hydroxy-3-(4-methoxy-3-methyl-phenyl)-1-methyl-1H-pyrazole 9.3 g.

후처리

  1. distillationThe toluene was distilled off
  2. additionAt room temperature, to the reaction mixture was added water 100 ml
  3. stirringwas stirred for three hours
  4. filtrationThe precipitates were filtered
  5. washwere washed with water 400 ml and ethyl acetate 500 ml
  6. customwere dried under reduced pressure

출처 및 근거

ORD 기록
ord-aefca471f2ed4c7198f8c8a9df217573
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09314023B2

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