2-(Ethoxymethylene)propanedinitrile → 5-amino-1-tert-butyl-1H-pyrazole-4-carbonitrile

HRID 1736570ノート

反応式

HRID 1736570 の反応式
[C:1]([NH:5][NH2:6])([CH3:4])([CH3:3])[CH3:2].C[O-].[Na+].C(O[CH:13]=[C:14]([C:17]#[N:18])[C:15]#[N:16])C>C(O)C>[C:1]([N:5]1[C:17]([NH2:18])=[C:14]([C:15]#[N:16])[CH:13]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 671522-(Ethoxymethylene)propanedinitrileHCID 81890tert-ButylhydrazineHCID 10942334Sodium Methoxide

生成物 1

HCID 27974545-amino-1-tert-butyl-1H-pyrazole-4-carbonitrile収率 87.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a mixture of tert-butylhydrazine (40 g, 0.32 mol), sodium methoxide (18 g, 0.32 mol) and ethanol 150 ml) was added ethoxymethylene malononitrile (42 g, 0.32 mol). The reaction mixture was heated to reflux for 2 hours and the solvent was removed in vacuo. The residue was extracted with chloroform, washed with water and the organic layer was concentrated in vacuo to afford 46 g (87%) of 1-tert-butyl-5-amino-1H-pyrazole-4-carbonitrile as a semi-solid.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 2 hours
  3. customthe solvent was removed in vacuo
  4. extractionThe residue was extracted with chloroform
  5. washwashed with water
  6. concentrationthe organic layer was concentrated in vacuo

出典と根拠

ORDレコード
ord-c815d297dd404e33ac24f2dffda46db9
出典データセット
uspto-grants-1996_07
特許番号
US05541187

反応ノート

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