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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
ノート
印刷プレビュー

反応式

HRID 1835151 の反応式
[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
参加物反応条件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 23503264Diethyl 1-(1-naphthalenylmethyl)pyrrole-3,4-dicarboxylate

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
200 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d616436f19a0493ab55b9218d141bc9f
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06770646B2

反応ノート

読み込み中…

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