Potassium Carbonate → 3'-fluoro-4'-[(4-methyl-6-oxo-2-propylpyrimidin-1(6H)-yl)methyl]biphenyl-2-carbonitrile

HRID 1674311노트

반응식

HRID 1674311 반응식
[CH3:1][C:2]1[N:7]=[C:6]([CH2:8][CH2:9][CH3:10])[NH:5][C:4](=[O:11])[CH:3]=1.Br[CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[C:21]([C:26]#[N:27])=[CH:22][CH:23]=[CH:24][CH:25]=2)=[CH:16][C:15]=1[F:28].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[F:28][C:15]1[CH:16]=[C:17]([C:20]2[C:21]([C:26]#[N:27])=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:18]=[CH:19][C:14]=1[CH2:13][N:5]1[C:4](=[O:11])[CH:3]=[C:2]([CH3:1])[N:7]=[C:6]1[CH2:8][CH2:9][CH3:10]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 574600744'-(Bromomethyl)-3'-fluorobiphenyl-2-carbonitrileHCID 1355166076-methyl-2-propylpyrimidin-4(3H)-one

생성물 1

HCID 574609673'-fluoro-4'-[(4-methyl-6-oxo-2-propylpyrimidin-1(6H)-yl)methyl]biphenyl-2-carbonitrile수율 29.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
50 °C

실험 절차

To a solution of 6-methyl-2-propylpyrimidin-4(3H)-one (2.0 g) and 4′-(bromomethyl)-3′-fluorobiphenyl-2-carbonitrile (4.4 g) in acetonitrile (50 mL) was added potassium carbonate (3.6 g), and the mixture was stirred at 50° C. for 12 hr. The insoluble material was filtered off, the filtrate was concentrated, and the residue was purified by silica gel column chromatography to give the title compound (1.4 g, 29%) as a colorless viscous substance.

후처리

  1. filtrationThe insoluble material was filtered off
  2. concentrationthe filtrate was concentrated
  3. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-8429bcaf9e434f3baa779f6d08a56709
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998968B2

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