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Triethylamine → Methyl (R)-3-(N-Cyclobutyl-N-isopropylamino)-8-fluoro-3,4-dihydro-2H-1-benzopyran-5-carboxylate

HRID 1738322
Notes
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Reaction equation

HRID 1738322 reaction equation
[CH:1]1([N:5]([C@@H:9]2[CH2:14][C:13]3[C:15](OS(C(F)(F)F)(=O)=O)=[CH:16][CH:17]=[C:18]([F:19])[C:12]=3[O:11][CH2:10]2)[CH:6]([CH3:8])[CH3:7])[CH2:4][CH2:3][CH2:2]1.[C]=O.C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(N(CC)CC)C.CN([CH:69]=[O:70])C.[CH3:71][OH:72]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH:1]1([N:5]([C@@H:9]2[CH2:14][C:13]3=[C:15]([C:71]([O:70][CH3:69])=[O:72])[CH:16]=[CH:17][C:18]([F:19])=[C:12]3[O:11][CH2:10]2)[CH:6]([CH3:8])[CH3:7])[CH2:4][CH2:3][CH2:2]1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 8471TriethylamineHCID 812191,3-Bis(diphenylphosphino)propaneHCID 21901440N,N-dimethylformamide methanolHCID 54082177(R)-3-(N-Cyclobutyl-N-isopropylamino)-8-fluoro-5-trifluoromethylsulfonyloxy-3,4-dihydro-2H-1-benzopyranHCID 178418416HCID 178418416, compound

Product 1

HCID 53695439
Methyl (R)-3-(N-Cyclobutyl-N-isopropylamino)-8-fluoro-3,4-dihydro-2H-1-benzopyran-5-carboxylate
Yield 92%

Reagents, catalysts & solvents 1

HCID 167845palladium(II) acetateCatalyst

Conditions

Temperature
70 °C

Procedure

(R)-3-(N-Cyclobutyl-N-isopropylamino)-8-fluoro-5-trifluoromethylsulfonyloxy-3,4-dihydro-2H-1-benzopyran (1.65 g, 4.01 mmol) was dissolved in a solution of DMF/methanol (6:2, 30 mL) and then degassed followed by the inlet of carbon monoxide (×3). With a slight positive pressure of carbon monoxide, palladium(II)-acetate (30 mg), 1,3-bis(diphenylphosphino)propane (55 mg) and triethylamine (1.25 mL, 8.8 mmol) were added and the reaction mixture was degassed and subjected to carbon monoxide once again. The reaction was heated to 70° C. under carbon monoxide atmosphere with vigorous stirring for 6 h. The reaction was allowed to cool and the solvent was removed in vacuo. The remains were taken into a 2M solution of NH3 and then extracted, twice, with diethyl ether. The combined ether portions were dried (MgSO4), filtered, and the solvent removed in vacuo to give the crude residue. Chromatography on silica (eluent: 8% ethyl acetate/hexane) gave 1.18 mg (92% yield) of the title compound as a clear oil. [α]21D =-139.1° (C=0.1; CHCl3). GC-MS (70 eV) M=321 (3%).

Workup

  1. customdegassed
  2. customthe reaction mixture was degassed
  3. temperatureto cool
  4. customthe solvent was removed in vacuo
  5. extractionextracted
  6. dry with materialThe combined ether portions were dried (MgSO4)
  7. filtrationfiltered
  8. customthe solvent removed in vacuo
  9. customto give the crude residue

Sources & evidence

ORD record
ord-47739388784340e198437b62b867618a
Source dataset
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05962514

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes