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Hydrochloric Acid → US10385022, Example 16

HRID 877977
Notes
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Reaction equation

HRID 877977 reaction equation
I[C:2]1[N:7]=[CH:6][C:5]([N:8]([CH3:25])[C:9](=[O:24])[C:10]2[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[C:12]([C:20]([F:23])([F:22])[F:21])[CH:11]=2)=[C:4]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[CH3:32])[CH:3]=1.CC(C)([O-])C.[Na+].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.C(=[NH:98])(C1C=CC=CC=1)C1C=CC=CC=1.Cl.C([O-])(O)=O.[Na+]>C1(C)C=CC=CC=1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[NH2:98][C:2]1[N:7]=[CH:6][C:5]([N:8]([CH3:25])[C:9](=[O:24])[C:10]2[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[C:12]([C:20]([F:23])([F:22])[F:21])[CH:11]=2)=[C:4]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[CH3:32])[CH:3]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

9

Reactant 6

HCID 313Hydrochloric AcidHCID 136809Benzophenone imineHCID 516892Sodium BicarbonateHCID 634876Binap, (A+-)-HCID 23676156Sodium t-butoxideHCID 86670689N-(6-Iodo-4-o-tolylpyridin-3-yl)-N-methyl-3,5-bis(trifluoromethyl)benzamide

Product 1

HCID 86670688US10385022, Example 16Yield 35%

Reagents, catalysts & solvents 2

HCID 167845palladium(II) acetateCatalystHCID 1140TolueneSolvent

Conditions

Temperature
150 °C

Procedure

N-(6-Iodo-4-o-tolylpyridin-3-yl)-N-methyl-3,5-bis(trifluoromethyl)benzamide (60 mg, 0.11 mmol), sodium tert-butoxide (31 mg, 0.32 mmol), palladium acetate (2.4 mg, 0.011 mmol, CAS RN 3375-31-3) and BINAP (19.9 mg; 0.032 mmol, CAS RN 76189-55-4) were dissolved in toluene (4 mL) and stirred under an argon atmosphere for 10 min. Benzophenone imine (38 mg, 0.21 mmol, CAS RN 1013-88-3) was added and the reaction mixture was sealed and heated to 150° C. by microwave irradiation for 30 minutes. The reaction mixture was cooled, unsealed and 200 μL of 1M aqueous HCl was added. After stirring for 1 h, the reaction mixture was neutralized with saturated aqueous NaHCO3 solution and extracted three times with EtOAc. The combined organic layers were washed with brine and dried over MgSO4. Filtration followed by removal of volatiles under reduced pressure afforded a brown solid. Column chromatography on silica gel (50% EtOAc in n-hexane) afforded the title compound as a yellow solid (17 mg, 35%). MS (ESI): m/z=453.9 [M+H]+.

Workup

  1. customthe reaction mixture was sealed
  2. temperatureThe reaction mixture was cooled
  3. stirringAfter stirring for 1 h
  4. extractionextracted three times with EtOAc
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationFiltration
  8. customfollowed by removal of volatiles under reduced pressure
  9. customafforded a brown solid

Sources & evidence

ORD record
ord-ed30ed93653040aab2f5f55b2cdc3d7d
Source dataset
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08987307B2

Reaction notes

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