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Ammonium Chloride → 7-Fluoro-5-methyl-1H-indole

HRID 2354278
Notes
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Reaction equation

HRID 2354278 reaction equation
[F:1][C:2]1[CH:3]=[C:4]([CH3:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-])=O.[CH:12]([Mg]Br)=[CH2:13].[Cl-].[NH4+]>O1CCCC1>[F:1][C:2]1[CH:3]=[C:4]([CH3:11])[CH:5]=[C:6]2[C:7]=1[NH:8][CH:13]=[CH:12]2
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 25517Ammonium ChlorideHCID 67966Benzene, 2-fluoro-4-methyl-1-nitro-HCID 178418507HCID 178418507, compound

Product 1

HCID 218747727-Fluoro-5-methyl-1H-indole

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a solution of 3-fluoro-4-nitrotoluene (3.1 g) in tetra hydrofuran (160 mL) was added vinyl magnesium bromide (1.0 mol/L tetra hydrofuran solution, 60.0 mL) at −40° C., and the mixture was stirred at the same temperature for 1 hour. To the mixture was added a saturated aqueous ammonium chloride solution, and the resulting mixture was stirred at room temperature for 1 hour. The mixture was extracted with diethyl ether. The extract was washed with a saturated aqueous ammonium chloride solution, water and brine successively, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on amino-propylated silica gel (eluent: n-hexane/ethyl acetate=19/1-4/1) to give 7-fluoro-5-methyl-1H-indole (0.96 g). The title compound was prepared in a similar manner to that described in Reference Example 1 using this material instead of 4-methyl-1H-indole.

Workup

  1. stirringthe resulting mixture was stirred at room temperature for 1 hour
  2. extractionThe mixture was extracted with diethyl ether
  3. washThe extract was washed with a saturated aqueous ammonium chloride solution, water and brine successively
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was purified by column chromatography on amino-propylated silica gel (eluent: n-hexane/ethyl acetate=19/1-4/1)

Sources & evidence

ORD record
ord-3f0f7fbb62f94b1789c54a67b2579b84
Source dataset
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07750145B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes