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Hydrochloric Acid → 2-(Ethylsulfanyl)-4-oxo-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,4-dihydropyrido[2,3-d]pyrimidine-7-carboxamide

HRID 570725
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HRID 570725 반응식
[CH2:1]([S:3][C:4]1[N:5]([C:17]2[CH:22]=[CH:21][C:20]([O:23][CH2:24][C:25]([F:28])([F:27])[F:26])=[CH:19][CH:18]=2)[C:6](=[O:16])[C:7]2[CH:13]=[CH:12][C:11]([CH:14]=[O:15])=[N:10][C:8]=2[N:9]=1)[CH3:2].CC(=CC)C.P([O-])(O)(O)=O.[K+].Cl([O-])=O.[Na+].Cl.[NH4+].O[N:47]1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C>CN(C)C=O.O.CC(O)(C)C.O>[CH2:1]([S:3][C:4]1[N:5]([C:17]2[CH:22]=[CH:21][C:20]([O:23][CH2:24][C:25]([F:27])([F:28])[F:26])=[CH:19][CH:18]=2)[C:6](=[O:16])[C:7]2[CH:13]=[CH:12][C:11]([C:14]([NH2:47])=[O:15])=[N:10][C:8]=2[N:9]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 7

HCID 313Hydrochloric AcidHCID 105532-Methyl-2-buteneHCID 516951Monobasic potassium phosphateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 220338091-Hydroxybenzotriazole, ammonium saltHCID 23668197Sodium Chlorite
HCID 86685385
2-(Ethylsulfanyl)-4-oxo-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,4-dihydropyrido[2,3-d]pyrimidine-7-carbaldehyde

생성물 1

HCID 680153212-(Ethylsulfanyl)-4-oxo-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,4-dihydropyrido[2,3-d]pyrimidine-7-carboxamide수율 25.3%

시약·촉매·용매 3

HCID 962Water용매2회HCID 6228Dimethylformamide용매HCID 714019492-Methylpropan-2-ol--water (1/1)용매

실험 절차

To a mixture of 2-(ethylsulfanyl)-4-oxo-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,4-dihydropyrido[2,3-d]pyrimidine-7-carbaldehyde (299 mg), 2-methylbut-2-ene (387 mg), potassium dihydrogen phosphate (88 mg) and 2-methyl-2-propanol/water (4/1, 70 ml) was added sodium chlorite (232 mg) by small portions, and the mixture was stirred at room temperature for 1 hr. To the reaction mixture were added 1M hydrochloric acid and water under ice-cooling, and the mixture was extracted with tetrahydrofuran. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give a pale-yellow residue. The residue (117 mg) and 1-hydroxybenzotriazole ammonium (40 mg) were dissolved in N,N-dimethylformamide (2 ml), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (56 mg) was added thereto, and the mixture was stirred at room temperature for 16 hr. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The extract was washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane) and then (NH, ethyl acetate/hexane), and recrystallized from a mixed solvent of ethyl acetate/hexane to give the white title compound (28 mg).

후처리

  1. temperaturecooling
  2. extractionthe mixture was extracted with tetrahydrofuran
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give a pale-yellow residue
  7. stirringthe mixture was stirred at room temperature for 16 hr
  8. extractionthe mixture was extracted with ethyl acetate
  9. washThe extract was washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine
  10. dry with materialdried over anhydrous magnesium sulfate
  11. customthe solvent was evaporated under reduced pressure
  12. customThe obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane)
  13. custom(NH, ethyl acetate/hexane), and recrystallized from a mixed solvent of ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-e8b765ec18d1422a8925b752f5f3b04f
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09023858B2

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