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

HRID 2071642노트

반응식

HRID 2071642 반응식
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

참가 물질

5

반응물 3

HCID 241BenzeneHCID 12315N-MethylpropylamineHCID 22756855HCID 22756855, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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°.

후처리

  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°

출처 및 근거

ORD 기록
ord-5015d849e73641948321aeec7aa0aef8
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04048184

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