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dimethyl-(5-nitro-1H-inden-2-yl)-amine → N,N-Dimethyl-5-nitro-2-indanamine

HRID 1881362
Notes
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Reaction equation

HRID 1881362 reaction equation
[CH3:1][N:2]([CH3:15])[C:3]1[CH2:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([N+:12]([O-:14])=[O:13])=[CH:7][CH:6]=2>CO.C1COCC1.[Pd]>[CH3:1][N:2]([CH3:15])[CH:3]1[CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([N+:12]([O-:14])=[O:13])[CH:9]=2)[CH2:4]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 1

HCID 68752984dimethyl-(5-nitro-1H-inden-2-yl)-amine

Product 1

HCID 25138868N,N-Dimethyl-5-nitro-2-indanamineYield 82.1%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 21899815MeOH tetrahydrofuranSolvent

Procedure

To a solution of 5-nitro-2-indanone (885 mg, 5 mmol) in THF (15 mL) was added dimethylamine (2N in THF, 5 mL, 10 mmol) dropwise. The reaction mixture was stirred at r.t. for 5 h. Water was added and the reaction mixture was extracted with EtOAc. Combined organic layers were washed with water and brine and dried over Na2SO4. The concentrated crude product was filtered through a short pad of silica gel (EtOAc:hexane=1:1) and the filtrate was concentrated to give dimethyl-(5-nitro-1H-inden-2-yl)-amine as a dark red solid (1.0 g, 98%). Dimethyl-(5-nitro-1H-inden-2-yl)-amine (1.0 g, 4.9 mmol) was hydrogenated using Pd/C (10% dry, ca. 300 mg) and H2 in MeOH:THF (1:1, 30 mL) at 1 atm at r.t. for 5 h. The reaction mixture was filtered through a pad of celite and the filtrate was concentrated. The concentrated filtrate was further purified via short silica gel column chromatography (EtOAc: MeOH=6:4) to give the title compound as a yellow solid (830 mg, 82%).

Workup

  1. customat r.t.
  2. customfor 5 h
  3. filtrationThe reaction mixture was filtered through a pad of celite
  4. concentrationthe filtrate was concentrated
  5. customThe concentrated filtrate was further purified via short silica gel column chromatography (EtOAc: MeOH=6:4)

Sources & evidence

ORD record
ord-51bc9aaea7ec4580b58183c8e5f3b6a6
Source dataset
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08318790B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes