2-Chloropyrimidine → HCID 19785323, 화합물

HRID 256671

반응식

HRID 256671 반응식
Cl[C:2]1[N:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[NH2:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][CH:14]([NH:17][C:18]2[N:19]([CH2:27][C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)[C:20]3[C:25]([N:26]=2)=[CH:24][N:23]=[CH:22][N:21]=3)[CH2:13][CH2:12]1.C(=O)([O-])O.[Na+]>C(O)C>[F:34][C:31]1[CH:30]=[CH:29][C:28]([CH2:27][N:19]2[C:18]([NH:17][CH:14]3[CH2:13][CH2:12][N:11]([CH2:10][CH2:9][NH:8][C:2]4[N:7]=[CH:6][CH:5]=[CH:4][N:3]=4)[CH2:16][CH2:15]3)=[N:26][C:25]3[C:20]2=[N:21][CH:22]=[N:23][CH:24]=3)=[CH:33][CH:32]=1

참가 물질

5

반응물 3

HCID 744042-ChloropyrimidineHCID 516892Sodium BicarbonateHCID 19785318N-[1-(2-aminoethyl)-4-piperidinyl]-9-[(4-fluorophenyl)methyl]-9H-purin-8-amine

생성물 1

HCID 19785323HCID 19785323, 화합물수율 67%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1.7 parts of 2-chloropyrimidine, 5.5 parts of N-[1-(2 aminoethyl)-4-piperidinyl]-9-[(4-fluorophenyl)methyl]-9H-purin-8-amine, 1.5 parts of sodium hydrogen carbonate and 160 parts of ethanol was stirred and refluxed for 20 hours. The reaction mixture was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from acetonitrile, yielding 4.5 parts (67%) of 9-[(4-fluorophenyl)methyl]-N-[1-[2-(2-pyrimidinylamino)ethyl]-4-piperidinyl]-9H-purin-8-amine; mp. 164.1° C. (compound 164).

후처리

  1. temperaturerefluxed for 20 hours
  2. customThe reaction mixture was evaporated
  3. customThe residue was purified by column chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
  5. customThe pure fractions were collected
  6. customthe eluent was evaporated
  7. customThe residue was crystallized from acetonitrile

출처 및 근거

ORD 기록
ord-547c46afb598489a92369f1f60ef5336
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258380

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