1,1'-Carbonyldiimidazole → 6-Bromo-3-(2-(4-methylpiperazin-1-yl)ethyl)-3,4-dihydropyrido[2,3-d]pyrimidin-2(1H)-one

HRID 633977

반응식

HRID 633977 반응식
C1N=CN([C:6](N2C=NC=C2)=[O:7])C=1.[Br:13][C:14]1[CH:15]=[C:16]([CH2:21][NH:22][CH2:23][CH2:24][N:25]2[CH2:30][CH2:29][N:28]([CH3:31])[CH2:27][CH2:26]2)[C:17]([NH2:20])=[N:18][CH:19]=1>O1CCOCC1>[Br:13][C:14]1[CH:19]=[N:18][C:17]2[NH:20][C:6](=[O:7])[N:22]([CH2:23][CH2:24][N:25]3[CH2:30][CH2:29][N:28]([CH3:31])[CH2:27][CH2:26]3)[CH2:21][C:16]=2[CH:15]=1

참가 물질

4

반응물 2

HCID 682631,1'-CarbonyldiimidazoleHCID 671545225-Bromo-3-((2-(4-methylpiperazin-1-yl)ethylamino)methyl)pyridin-2-amine

생성물 1

HCID 671546046-Bromo-3-(2-(4-methylpiperazin-1-yl)ethyl)-3,4-dihydropyrido[2,3-d]pyrimidin-2(1H)-one

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

CDI (815 mg, 5.0 mmol) was added to a solution of 5-bromo-3-((2-(4-methylpiperazin-1-yl)ethylamino)methyl)pyridin-2-amine (550 mg, 1.67 mmol) in dioxane (13 mL). The reaction mixture was stirred overnight at reflux. After concentration to dryness, the residue was purified by chromatography on silica gel using dichloromethane/methanol/ammoniac (10:0:0.1 to 9:1:0.1) as eluent. The title product was obtained as a yellow solid (430 mg, 72%).

후처리

  1. temperatureat reflux
  2. concentrationAfter concentration to dryness
  3. customthe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-45840ed07c4f4489b3b53763010e5a61
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321769B2

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