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Methylamine → (5-Chloro-3-methyl-benzo[b]thiophen-2-ylmethyl)methylamine

HRID 1362040
Notes
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Reaction equation

HRID 1362040 reaction equation
[Cl:1][C:2]1[CH:13]=[CH:12][C:5]2[S:6][C:7]([CH:10]=O)=[C:8]([CH3:9])[C:4]=2[CH:3]=1.[CH3:14][NH2:15].[BH4-].[Na+]>CO>[Cl:1][C:2]1[CH:13]=[CH:12][C:5]2[S:6][C:7]([CH2:10][NH:15][CH3:14])=[C:8]([CH3:9])[C:4]=2[CH:3]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 6329MethylamineHCID 36596315-Chloro-3-methylbenzo[b]thiophene-2-carbaldehydeHCID 4311764Sodium borohydride

Product 1

HCID 66966971(5-Chloro-3-methyl-benzo[b]thiophen-2-ylmethyl)methylamine

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To 5-chloro-3-methyl-benzo[b]thiophene-2-carbaldehyde (5.10 g, 24.2 mmol) was added a solution of 2 M methylamine in methanol (81 mL) and the resulting mixture was stirred overnight at room temperature. The mixture was concentrated under reduced pressure and the residue taken up in ethanol (81 mL). The solution was cooled to 0° C., NaBH4 (1.37 g, 36.3 mmol) was added in one portion, and stirring was continued overnight. The mixture was concentrated under reduced pressure and the residue was combined with 1 M NaOH (200 mL). The mixture was extracted with diethyl ether (3×150 mL). The combined organics were washed with brine (100 mL), dried over Na2SO4, filtered and concentrated under reduced pressure to the title compound (4.83 g, 88%) as a pale yellow oil which crystallized under vacuum: 1H NMR (300 MHz, CDCl3) δ 7.69-7.59 (m, 2H), 7.25 (m, 1H), 3.96 (s, 2H), 2.50 (s, 3H), 2.31 (s, 3H).

Workup

  1. concentrationThe mixture was concentrated under reduced pressure
  2. temperatureThe solution was cooled to 0° C.
  3. stirringstirring
  4. waitwas continued overnight
  5. concentrationThe mixture was concentrated under reduced pressure
  6. extractionThe mixture was extracted with diethyl ether (3×150 mL)
  7. washThe combined organics were washed with brine (100 mL)
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure to the title compound (4.83 g, 88%) as a pale yellow oil which
  11. customcrystallized under vacuum

Sources & evidence

ORD record
ord-b8b7998adf4c4ce0b29cdb320494e206
Source dataset
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07879872B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes