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Dimethylformamide → Methyl 2-(4-tert-butylthiazol-2-yl)benzofuran-5-carboxylate

HRID 1604648
Notes
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Reaction equation

HRID 1604648 reaction equation
[C]=O.FC(F)(F)S(O[C:9]1[CH:10]=[CH:11][C:12]2[O:16][C:15]([C:17]3[S:18][CH:19]=[C:20]([C:22]([CH3:25])([CH3:24])[CH3:23])[N:21]=3)=[CH:14][C:13]=2[CH:26]=1)(=O)=O.C1(OP(CCCP([O:57][C:58]2C=CC=CC=2)(OC2C=CC=CC=2)=O)(OC2C=CC=CC=2)=O)C=CC=CC=1.C(N(CC)CC)C.CN(C)[CH:73]=[O:74]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CO>[C:22]([C:20]1[N:21]=[C:17]([C:15]2[O:16][C:12]3[CH:11]=[CH:10][C:9]([C:73]([O:57][CH3:58])=[O:74])=[CH:26][C:13]=3[CH:14]=2)[S:18][CH:19]=1)([CH3:25])([CH3:24])[CH3:23]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 5

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 196036842-(4-Tert-butylthiazol-2-yl)benzofuran-5-yl trifluoromethanesulfonateHCID 538511551,3-Bis(diphenylphosphono)propaneHCID 178418416HCID 178418416, compound

Product 1

HCID 19603836
Methyl 2-(4-tert-butylthiazol-2-yl)benzofuran-5-carboxylate

Reagents, catalysts & solvents 2

HCID 167845palladium(II) acetateCatalystHCID 887MethanolSolvent

Conditions

Temperature
70 °C

Procedure

Carbon monoxide was introduced by bubbling to a mixture of 2-(4-tert-butylthiazol-2-yl)benzofuran-5-yl trifluoromethanesulfonate (6.0 g), palladium acetate (99.7 mg), 1,3-bis(diphenylphosphono)propane (183 mg, 0.44 mmol) and triethylamine (4.13 ml) in a mixed solvent of methanol (15 ml) and N,N-dimethylformamide (30 ml) at room temperature for 1 hour. The mixture was warmed to 70° C. and stirred under carbon monoxide balloon for 3 hours. The resulting mixture was filtered through celite and the residue was washed with ethyl acetate. The filtrate and washing solution was combined and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel using ethyl acetate-n-hexane as eluent to give methyl 2-(4-tert-butylthiazol-2-yl)benzofuran-5-carboxylate (3.92 g) as a colorless powder.

Workup

  1. filtrationThe resulting mixture was filtered through celite
  2. washthe residue was washed with ethyl acetate
  3. washThe filtrate and washing solution
  4. customevaporated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel

Sources & evidence

ORD record
ord-438352edabd341d88dfbc1795d420f22
Source dataset
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05994378

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes