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Sodium Hydroxide → 3-[({4-[(cyclohexyl{5-[(1,1-dioxidotetrahydro-2H-thiopyran-4-yl)oxy]-3-methyl-1-benzofuran-2-yl}methyl)amino]phenyl}carbonyl)(methyl)amino]propanoic acid

HRID 2091409
Notes
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Reaction equation

HRID 2091409 reaction equation
[CH:1]1([CH:7]([NH:19][C:20]2[CH:25]=[CH:24][C:23]([C:26]([N:28]([CH3:36])[CH2:29][CH2:30][C:31]([O:33]CC)=[O:32])=[O:27])=[CH:22][CH:21]=2)[C:8]2[O:9][C:10]3[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][C:11]=3[C:12]=2[CH3:13])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CC1C=CC(S(O[CH:48]2[CH2:53][CH2:52][S:51](=[O:55])(=[O:54])[CH2:50][CH2:49]2)(=O)=O)=CC=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].[OH-].[Na+]>CN(C)C=O.C(O)C.O1CCCC1.O>[CH:1]1([CH:7]([NH:19][C:20]2[CH:25]=[CH:24][C:23]([C:26]([N:28]([CH3:36])[CH2:29][CH2:30][C:31]([OH:33])=[O:32])=[O:27])=[CH:22][CH:21]=2)[C:8]2[O:9][C:10]3[CH:17]=[CH:16][C:15]([O:18][CH:48]4[CH2:53][CH2:52][S:51](=[O:55])(=[O:54])[CH2:50][CH2:49]4)=[CH:14][C:11]=3[C:12]=2[CH3:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

9

Reactant 4

HCID 14798Sodium HydroxideHCID 62657Potassium Phosphate, Tribasic2×HCID 594258721,1-dioxidotetrahydro-2H-thiopyran-4-yl 4-methylbenzenesulfonate2×HCID 66777718HCID 66777718, compound

Product 1

HCID 66778289
3-[({4-[(cyclohexyl{5-[(1,1-dioxidotetrahydro-2H-thiopyran-4-yl)oxy]-3-methyl-1-benzofuran-2-yl}methyl)amino]phenyl}carbonyl)(methyl)amino]propanoic acid
Yield 29%

Reagents, catalysts & solvents 4

HCID 702EthanolSolventHCID 962WaterSolventHCID 6228DimethylformamideSolventHCID 8028TetrahydrofuranSolvent

Conditions

Temperature
100 °C

Procedure

A solution of ethyl 3-{[(4-{[cyclohexyl(5-hydroxy-3-methyl-1-benzofuran-2-yl)methyl]amino}phenyl)carbonyl](methyl)amino}propanoate (400 mg) obtained in Example A194(4), 1,1-dioxidotetrahydro-2H-thiopyran-4-yl 4-methylbenzenesulfonate (593 mg) synthesized above and tripotassium phosphate (223 mg) in N,N-dimethylformamide (4 mL) was stirred at 100° C. for 14 hr. 1,1-Dioxidotetrahydro-2H-thiopyran-4-yl 4-methylbenzenesulfonate (593 mg) and tripotassium phosphate (112 mg) were further added to the mixture, and the mixture was stirred at 100° C. for 2 hr then at 120° C. for 3 hr. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. After filtration, the filtrate was concentrated. The residue was subjected to silica gel column chromatography (hexane-ethyl acetate 100:0-34:66, v/v) to give a colorless amorphous form (200 mg). The colorless amorphous form (200 mg) was dissolved in ethanol (1.5 mL) and tetrahydrofuran (1.5 mL), and 1N aqueous sodium hydroxide solution (0.64 mL) was added to the solution, and the mixture was stirred at room temperature for 30 min. The solvent was evaporated under reduced pressure, water (4 mL) was added to the residue, and the mixture was neutralized with 1N hydrochloric acid (0.64 mL) under ice-cooling and stirred at 0° C. for 30 min. The resulting precipitate was collected by filtration, and dried to give the title compound (136 mg, 29%) as a colorless amorphous form.

Workup

  1. stirringthe mixture was stirred at 100° C. for 2 hr
  2. waitat 120° C. for 3 hr
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationAfter filtration
  7. concentrationthe filtrate was concentrated
  8. customv/v) to give a colorless amorphous form (200 mg)
  9. stirringthe mixture was stirred at room temperature for 30 min
  10. customThe solvent was evaporated under reduced pressure, water (4 mL)
  11. additionwas added to the residue
  12. temperaturecooling
  13. stirringstirred at 0° C. for 30 min
  14. filtrationThe resulting precipitate was collected by filtration
  15. customdried

Sources & evidence

ORD record
ord-ddbc6fb2ef024355a1a6c0b3b8c7a92a
Source dataset
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08436043B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes