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Methylhydrazine → 2,3-Dihydro-2-methyl-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazin-1,4(6H)-dione

HRID 1835151
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HRID 1835151 반응식
[CH3:1][NH:2][NH2:3].[C:4]1([CH2:14][N:15]2[CH:19]=[C:18]([C:20](OCC)=[O:21])[C:17]([C:25](OCC)=[O:26])=[CH:16]2)[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1>C(O)C>[CH3:1][N:2]1[C:25](=[O:26])[C:17]2=[CH:16][N:15]([CH2:14][C:4]3[C:13]4[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=4)[CH:7]=[CH:6][CH:5]=3)[CH:19]=[C:18]2[C:20](=[O:21])[NH:3]1
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참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 23503264Diethyl 1-(1-naphthalenylmethyl)pyrrole-3,4-dicarboxylate

생성물 1

HCID 235032482,3-Dihydro-2-methyl-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazin-1,4(6H)-dione

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
200 °C

실험 절차

Methyl hydrazine (0.55 ml) was added to a solution of diethyl 1-(1-naphthalenylmethyl)pyrrole-3,4-dicarboxylate (1.00 g) in ethanol (10 ml). The mixture was heated at 200° C. in a sealed tube for 3 days. The mixture was evaporated and the residue was purified by column chromatography, eluting with ethyl acetate:methanol (19:1). The resulting solid was suspended in ethyl acetate (25 ml), heated to reflux, and allowed to cool to ambient temperature. The title compound (0.105 g) was collected by filtration.

후처리

  1. customThe mixture was evaporated
  2. customthe residue was purified by column chromatography
  3. washeluting with ethyl acetate:methanol (19:1)
  4. temperatureheated
  5. temperatureto reflux
  6. temperatureto cool to ambient temperature
  7. filtrationThe title compound (0.105 g) was collected by filtration

출처 및 근거

ORD 기록
ord-d616436f19a0493ab55b9218d141bc9f
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06770646B2

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