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Methylhydrazine → 5-amino-3-benzyl-1-methyl-1H-pyrazole-4-carbonitrile

HRID 1426275
ノート
印刷プレビュー

反応式

HRID 1426275 の反応式
CO[C:3](=[C:11]([C:14]#[N:15])[C:12]#[N:13])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[CH3:16][NH:17][NH2:18]>C(O)C>[NH2:13][C:12]1[N:17]([CH3:16])[N:18]=[C:3]([CH2:4][C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=2)[C:11]=1[C:14]#[N:15]
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 224493462-(1-Methoxy-2-phenylethylidene)propanedinitrile

生成物 1

HCID 679629765-amino-3-benzyl-1-methyl-1H-pyrazole-4-carbonitrile

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of (1-methoxy-2-phenylethylidene)malononitrile (prepared by the method of B. C. Kraybill et al., J. Am. Chem. Soc. 2002, 124, 12118-12128; 10 g, 50 mmol) and methylhydrazine (2.3 g, 50 mmol) in ethanol (120 mL) was heated to reflux for 10 minutes. The reaction was concentrated in vacuo, and the residue was diluted with water (200 mL) and extracted with EtOAc (3×100 mL). The combined organic layers were washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure to afford C10 as a yellow solid. Yield: 10 g, 47 mmol, 94%.

後処理

  1. customprepared by the method of B
  2. temperatureto reflux for 10 minutes
  3. concentrationThe reaction was concentrated in vacuo
  4. additionthe residue was diluted with water (200 mL)
  5. extractionextracted with EtOAc (3×100 mL)
  6. washThe combined organic layers were washed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customto afford C10 as a yellow solid

出典と根拠

ORDレコード
ord-c8441e974d314f01a0b7532e5a95c7c5
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08933095B2

反応ノート

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