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Aniline → Tert-butyl 2-benzoylindoline-1-carboxylate

HRID 1475910
Notes
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Reaction equation

HRID 1475910 reaction equation
[O:1]=[C:2]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:11][C:12](=[O:18])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15].CCCCCCCCCC.C(OO)(C)(C)C.NC1C=CC=CC=1>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C.CCCCCC.C(OCC)(=O)C.O>[C:2]([CH:3]1[CH2:4][C:5]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:11]1[C:12]([O:13][C:14]([CH3:17])([CH3:15])[CH3:16])=[O:18])(=[O:1])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

9

Reactant 4

HCID 6115AnilineHCID 6410tert-Butyl hydroperoxideHCID 15600DecaneHCID 68281220Tert-butyl 2-(3-oxo-3-phenylpropyl)phenylcarbamate

Product 1

HCID 68281223Tert-butyl 2-benzoylindoline-1-carboxylateYield 76%

Reagents, catalysts & solvents 4

HCID 67553
Tetrabutylammonium Iodide
Catalyst
HCID 962WaterSolvent
HCID 8857Ethyl AcetateSolvent
HCID 21226206Ethyl acetate hexaneSolvent

Procedure

A reactor was charged with 325 mg (1.0 mmol) of tert-butyl 2-(3-oxo-3-phenylpropyl)phenylcarbamate (an11) obtained in Synthesis Example 5, 36.9 mg (0.10 mmol) of tetrabutylammonium iodide (Bu4N+I−), and 50 mL of ethyl acetate as a solvent to prepare a solution. Subsequently, 364 μL of 5.5 M decane solution (manufactured by Aldrich) containing 2.0 mmol of tert-butyl hydroperoxide (TBHP) as an oxidizing agent was added to the solution in an amount corresponding to 2 equivalents based on the aniline derivative (an1). After adjusting the temperature of the reaction system to 50° C., the mixture was reacted for 10 hours with stirring. After cooling the reaction mixture including the reaction product to room temperature, the reaction mixture was added to 20 mL of water, and extracted twice with ethyl acetate. The resulting organic layer was sequentially washed with a saturated sodium sulfite (Na2SO3) aqueous solution, an NaCl aqueous solution, and water, followed by the addition of anhydrous sodium sulfate (Na2SO4). The solvent was then evaporated under reduced pressure to obtain a concentrate including a crude product. The concentrate was subjected to silica gel flash column chromatography (eluant: hexane/ethyl acetate=6/1) to obtain 246 mg (0.76 mmol) of tert-butyl 2-benzoylindoline-1-carboxylate represented by the formula (as1) (white solid). The yield was 76% (see Table 1-1). The analysis data for the resulting compound (as1) is shown below.

Workup

  1. customto prepare a solution
  2. additionwas added to the solution in an amount corresponding to 2 equivalents
  3. customto 50° C.
  4. customthe mixture was reacted for 10 hours
  5. temperatureAfter cooling the reaction mixture
  6. customto room temperature
  7. extractionextracted twice with ethyl acetate
  8. washThe resulting organic layer was sequentially washed with a saturated sodium sulfite (Na2SO3) aqueous solution
  9. additionan NaCl aqueous solution, and water, followed by the addition of anhydrous sodium sulfate (Na2SO4)
  10. customThe solvent was then evaporated under reduced pressure
  11. customto obtain a concentrate

Sources & evidence

ORD record
ord-4002ce25298f44ad9e6ed992f93e0a26
Source dataset
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09018394B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes