1-Butanol → 4-(4-Amino-phenyl)-1-methyl-1H-pyrazolo[3,4-c]pyridin-3-ylamine

HRID 1159451ノート

反応式

HRID 1159451 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:15]=[N:14][CH:13]=C(Cl)[C:9]=2[C:10]#[N:11])=[CH:4][CH:3]=1.[CH3:17][NH:18][NH2:19].[CH2:20](O)CCC>>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:15]=[N:14][CH:13]=[C:17]3[N:18]([CH3:20])[N:19]=[C:10]([NH2:11])[C:9]=23)=[CH:6][CH:7]=1

参加物

4

反応物 3

HCID 2631-ButanolHCID 6061MethylhydrazineHCID 451233613-(4-Aminophenyl)-5-chloroisonicotinonitrile

生成物 1

HCID 686444744-(4-Amino-phenyl)-1-methyl-1H-pyrazolo[3,4-c]pyridin-3-ylamine

実験手順

The product from Example 1C (150 mg, 0.65 mmol) and methylhydrazine (0.35 mL) in n-butanol (2 mL) was heated in a sealed vial at 190° C. for 30 minutes with stirring in a Smith Synthesizer microwave oven (at 300W). The reaction mixture was allowed to cool to room temperature and partitioned between water and ethyl acetate. The organic extract was dried (Na2SO4), filtered, and the filtrate was concentrated to provide 0.08 g of the title compound. MS (ESI(+)) m/e 240 (M+H)+.

後処理

  1. custompartitioned between water and ethyl acetate
  2. extractionThe organic extract
  3. dry with materialwas dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-dd4d95861b45473a84a5f97180212f45
出典データセット
uspto-grants-2010_10
特許番号
US07812166B2

反応ノート

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