Dimethylamine → HCID 70637790, compound

HRID 328139Notes

Reaction equation

HRID 328139 reaction equation
S(O[CH:12]1[CH2:30][CH2:29][N:15]2[C:16]3[CH:28]=[CH:27][CH:26]=[CH:25][C:17]=3[CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[CH:14]2[CH2:13]1)(C1C=CC(C)=CC=1)(=O)=O.[CH3:31][NH:32][CH3:33].O>CS(C)=O>[CH3:31][N:32]([CH3:33])[CH:12]1[CH2:30][CH2:29][N:15]2[C:16]3[CH:28]=[CH:27][CH:26]=[CH:25][C:17]=3[CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[CH:14]2[CH2:13]1

Participants

5

Reactant 3

HCID 674DimethylamineHCID 962WaterHCID 86734600HCID 86734600, compound

Product 1

HCID 70637790HCID 70637790, compound

Reagents, catalysts & solvents 1

HCID 679Dimethyl SulfoxideSolvent

Procedure

4 g of 2-tosyloxy-1,2,3,4,10,14b-hexahydro-pyridino[1,2-a] -dibenzo[ c,f]-azepine (eg.) are dissolved in 50 ml of dimethylsulphoxide. After that 15 ml of dimethylamine are added to the solution. This solution is now heated in a sealed ampoule on a vapour-bath for 2 hours. After cooling the solution, it is poured into 300 ml of water after which the mixture is extracted with 3×200 ml of ether. The ether layers are washed and then dried, whereupon the solvent is evaporated and the residue is recrystallized. Yield: 1.3 g.

Workup

  1. temperatureThis solution is now heated in a sealed ampoule on a vapour-bath for 2 hours
  2. temperatureAfter cooling the solution, it
  3. extractionis extracted with 3×200 ml of ether
  4. washThe ether layers are washed
  5. customdried, whereupon the solvent
  6. customis evaporated
  7. customthe residue is recrystallized

Sources & evidence

ORD record
ord-6399d703528d4fe18813adc66e93e119
Source dataset
uspto-grants-1977_04
Patent number
US04016161

Reaction notes

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