Benzene → 2-Methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]-pyridin-4-amine

HRID 65990ノート

反応式

HRID 65990 の反応式
Cl[C:2]1[C:3]2[C:4](=[N:14][N:15]([CH3:17])[CH:16]=2)[N:5]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:7]=1.C[NH:19][CH2:20][CH2:21][CH3:22].[CH:23]1C=CC=CC=1>CCOCC>[CH3:17][N:15]1[CH:16]=[C:3]2[C:4]([N:5]=[C:6]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH:7]=[C:2]2[NH:19][CH:20]([CH3:23])[CH2:21][CH3:22])=[N:14]1

参加物

5

反応物 3

HCID 241BenzeneHCID 12315N-MethylpropylamineHCID 22756855HCID 22756855、化合物

生成物 1

HCID 227568612-Methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]-pyridin-4-amine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

14.6 g. of 4-chloro-2-methyl-6-phenyl-2H-pyrazolo [3,4-b]pyridine (0.06 mol.) and a solution of 100 ml. of methylpropylamine in 150 ml. of benzene are heated at 220° in an autoclave for 20 hours. After cooling, the mixture is evaporated in vacuo, and to the residue 100 ml. of water and 100 ml. of chloroform are added. After agitation, the chloroform extract is separated and dried with Na2SO4. Evaporation yields an oily product which, after treatment with ether, becomes solid. 14.3 g. of 2-methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]pyridin-4-amine, (m.p. 148°-151° ), are recrystallized from ethyl acetate giving a pure product of the melting point 156°-157°.

後処理

  1. temperatureAfter cooling
  2. customthe mixture is evaporated in vacuo
  3. additionof chloroform are added
  4. extractionAfter agitation, the chloroform extract
  5. customis separated
  6. dry with materialdried with Na2SO4
  7. customEvaporation
  8. customyields an oily product which
  9. customof 2-methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]pyridin-4-amine, (m.p. 148°-151° ), are recrystallized from ethyl acetate giving a pure product of the melting point 156°-157°

出典と根拠

ORDレコード
ord-22d25771c50e412ea5e7d2f071eb77f4
出典データセット
uspto-grants-1978_12
特許番号
US04129738

反応ノート

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