2-Vinylpyridine → 9-[(4-fluorophenyl)methyl]-N-[1-[2-(2-pyridinyl)ethyl]-4-piperidinyl]-9H-purin-8-amine

HRID 2248821노트

반응식

HRID 2248821 반응식
[CH:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)=[CH2:2].[F:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][N:17]2[C:25]([NH:26][CH:27]3[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]3)=[N:24][C:23]3[C:18]2=[N:19][CH:20]=[N:21][CH:22]=3)=[CH:12][CH:11]=1>C(O)CCC>[F:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][N:17]2[C:25]([NH:26][CH:27]3[CH2:28][CH2:29][N:30]([CH2:2][CH2:1][C:3]4[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=4)[CH2:31][CH2:32]3)=[N:24][C:23]3[C:18]2=[N:19][CH:20]=[N:21][CH:22]=3)=[CH:12][CH:11]=1

참가 물질

4

반응물 2

HCID 75212-VinylpyridineHCID 197853439-[(4-fluorophenyl)methyl]-N-(4-piperidinyl)-9H-purin-8-amine

생성물 1

HCID 197853169-[(4-fluorophenyl)methyl]-N-[1-[2-(2-pyridinyl)ethyl]-4-piperidinyl]-9H-purin-8-amine수율 15%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A mixture of 1.93 parts of 2-ethenylpyridine, 5 parts of 9-[(4-fluorophenyl)methyl]-N-(4-piperidinyl)-9H-purin-8-amine and 80 parts of 1-butanol was stirred and refluxed overnight. The reaction mixture was evaporated. The residue was purified by column chromatography over silica gel using first a mixture of trichloromethane and methanol (95:5 by volume) and then a mixture of trichloromethane and methanol, saturated with ammonia (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from acetonitrile, yielding 1 part (15%) of 9-[(4-fluorophenyl)methyl]-N-[1-[2-(2-pyridinyl)ethyl]-4-piperidinyl]-9H-purin-8-amine; mp. 172.3° C. (compound 141).

후처리

  1. temperaturerefluxed overnight
  2. customThe reaction mixture was evaporated
  3. customThe residue was purified by column chromatography over silica gel using first
  4. additiona mixture of trichloromethane and methanol (95:5 by volume)
  5. additiona mixture of trichloromethane and methanol
  6. customThe pure fractions were collected
  7. customthe eluent was evaporated
  8. customThe residue was crystallized from acetonitrile

출처 및 근거

ORD 기록
ord-6c625de4514c4bda8102fb6eace99df8
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05041448

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