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Methylhydrazine → HCID 178488709、化合物

HRID 628532
ノート
印刷プレビュー

反応式

HRID 628532 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 178488709HCID 178488709、化合物収率 68%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aefca471f2ed4c7198f8c8a9df217573
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09314023B2

反応ノート

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