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

HRID 1736570노트

반응식

HRID 1736570 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c815d297dd404e33ac24f2dffda46db9
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05541187

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