Hydrazine hydrate (1:1) → 4-(4-Amino-phenyl)-1H-pyrazolo[3,4-c]pyridin-3-ylamine

HRID 1159449ノート

反応式

HRID 1159449 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:12](Cl)[C:9]=2[C:10]#[N:11])=[CH:4][CH:3]=1.O.[NH2:18][NH2:19]>>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:15]=[N:14][CH:13]=[C:12]3[NH:18][N:19]=[C:10]([NH2:11])[C:9]=23)=[CH:6][CH:7]=1

参加物

3

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 451233613-(4-Aminophenyl)-5-chloroisonicotinonitrile

生成物 1

HCID 671274914-(4-Amino-phenyl)-1H-pyrazolo[3,4-c]pyridin-3-ylamine

実験手順

The product from Example 1C (1.4 g) in hydrazine hydrate (10 mL) was heated at 110° C. for 3 hours, cooled to room temperature, and partitioned between water and ethyl acetate. The organic layer was dried (Na2SO4), filtered, and the filtrate was concentrated under reduced pressure. The residue was purified via silica gel chromatography eluting with 8% methanol in CH2Cl2 to provide 0.5 g of the title compound as a yellow solid. MS (ESI(+)) m/e 225 (M+H)+.

後処理

  1. custompartitioned between water and ethyl acetate
  2. dry with materialThe organic layer was dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified via silica gel chromatography
  6. washeluting with 8% methanol in CH2Cl2

出典と根拠

ORDレコード
ord-8812fa15ca2e4720b3569a0128ec1d38
出典データセット
uspto-grants-2010_10
特許番号
US07812166B2

反応ノート

読み込み中…