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Potassium Carbonate → 2-[3-{[(Tert-butoxycarbonyl)amino]methyl}-2-isobutyl-4-(4-methylphenyl)-6-quinolinyl]-1,3-thiazole-4-carboxylic acid

HRID 1986457
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HRID 1986457 반응식
[CH2:1]([C:5]1[C:14]([CH2:15][NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[C:13]([C:24]2[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=2)[C:12]2[C:7](=[CH:8][CH:9]=[C:10](OS(C(F)(F)F)(=O)=O)[CH:11]=2)[N:6]=1)[CH:2]([CH3:4])[CH3:3].[B].[C:40]([O-:43])(=[O:42])[CH3:41].[K+].Cl[C:46]1[S:47][CH:48]=C[N:50]=1.C(=O)([O-])[O-].[K+].[K+]>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].ClCCl.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O.C1(C)C=CC=CC=1.C(O)C.CS(C)=O>[C:19]([O:18][C:17]([NH:16][CH2:15][C:14]1[C:5]([CH2:1][CH:2]([CH3:3])[CH3:4])=[N:6][C:7]2[C:12]([C:13]=1[C:24]1[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=1)=[CH:11][C:10]([C:46]1[S:47][CH:48]=[C:41]([C:40]([OH:43])=[O:42])[N:50]=1)=[CH:9][CH:8]=2)=[O:23])([CH3:20])([CH3:21])[CH3:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

12

반응물 5

HCID 11430Potassium CarbonateHCID 764292-ChlorothiazoleHCID 517044Potassium AcetateHCID 5462311BoronHCID 510503433-{[(Tert-butoxycarbonyl)amino]methyl}-2-isobutyl-4-(4-methylphenyl)quinolin-6-yl trifluoromethanesulfonate

생성물 1

HCID 68829174
2-[3-{[(Tert-butoxycarbonyl)amino]methyl}-2-isobutyl-4-(4-methylphenyl)-6-quinolinyl]-1,3-thiazole-4-carboxylic acid
수율 36%

시약·촉매·용매 6

HCID 178418397HCID 178418397, 화합물촉매HCID 178418807HCID 178418807, 화합물촉매HCID 679Dimethyl Sulfoxide용매HCID 702Ethanol용매HCID 962Water용매3회HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

A mixture of tert-butyl [2-isobutyl-4-(4-methylphenyl)-6-trifluoromethanesulfonyloxy-quinolin-3-yl]methylcarbamate (0.50 g, 0.90 mmol), boron bispinacolate (0.25 g, 1.0 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium-dichloromethane (1:1) complex (0.020 g, 0.027 mmol), potassium acetate (0.27 g, 2.7 mmol) and dimethyl sulfoxide (20 ml) was stirred under an argon atmosphere at 100° C. for 15 min. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and a mixture of the residue, 2-chlorothiazole (0.17 g, 0.90 mmol), tetrakis(triphenylphosphine)palladium (0.10 g, 0.090 mmol), potassium carbonate (0.63 g, 4.5 mmol), ethanol (4 ml), toluene (20 ml) and water (4 ml) was stirred under an argon atmosphere at 100° C. for 17 hrs. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography. The obtained mixture was dissolved in tetrahydrofuran-methanol (1:1, 8 ml) and 1N aqueous sodium hydroxide solution (2 ml) was added. The mixture was stirred at room temperature for 15 min. 1N Hydrochloric acid (50 ml) was added to the reaction mixture and the mixture was extracted with ethyl acetate-tetrahydrofuran (1:1, 100 ml). The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography to give 2-[3-{[(tert-butoxycarbonyl)amino]methyl}-2-isobutyl-4-(4-methylphenyl)quinolin-6-yl]-1,3-thiazole-4-carboxylic acid (0.17 g, yield 36%) as pale-yellow crystals.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. stirringwas stirred under an argon atmosphere at 100° C. for 17 hrs
  6. extractionextracted with ethyl acetate
  7. washThe extract was washed with saturated brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customThe solvent was evaporated under reduced pressure
  10. customthe residue was purified by silica gel column chromatography
  11. dissolutionThe obtained mixture was dissolved in tetrahydrofuran-methanol (1:1, 8 ml)
  12. addition1N aqueous sodium hydroxide solution (2 ml) was added
  13. stirringThe mixture was stirred at room temperature for 15 min
  14. addition1N Hydrochloric acid (50 ml) was added to the reaction mixture
  15. extractionthe mixture was extracted with ethyl acetate-tetrahydrofuran (1:1, 100 ml)
  16. washThe extract was washed with saturated brine
  17. dry with materialdried over anhydrous magnesium sulfate
  18. customThe solvent was evaporated under reduced pressure
  19. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-6ca0e579954d4521afad167e0305055f
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07547710B2

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