Sodium Carbonate → HCID 13377596, compound

HRID 1703162Notes

Reaction equation

HRID 1703162 reaction equation
[CH3:1][C:2]1([CH3:17])[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=[C:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1.[CH2:18](O)[CH2:19][O:20][CH2:21][CH2:22][O:23][CH2:24][CH2:25][OH:26].C(O)C(O)CCl.C(=O)([O-])[O-].[Na+].[Na+]>CC(CC(C)C)=O>[CH3:1][C:2]1([CH3:17])[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=[C:11]1[CH2:16][CH2:15][N:14]([CH2:18][CH2:19][O:20][CH2:21][CH2:22][O:23][CH2:24][CH2:25][OH:26])[CH2:13][CH2:12]1

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 13377594HCID 13377594, compoundHCID 131712849HCID 131712849, compound

Product 1

HCID 13377596HCID 13377596, compound

Reagents, catalysts & solvents 1

HCID 7909Methyl Isobutyl KetoneSolvent

Procedure

2.5 g 4-(2,2-dimethyl-indane-1-ylidene)-piperidine, 1.95 g triethyleneglycol-monochlorhydrin and 2 g sodium carbonate in 50 ml methylisobutylketone are refluxed with stirring for 12 hours. After cooling, the reaction mixture is filtered and the filtrate evaporated. The residue is dissolved in ether, the solution washed two times with a little cold water, dried over sodium sulfate, filtered and evaporated, to give the title compound as a viscous oil. The neutral oxalate melts at 82°-85°.

Workup

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture is filtered
  3. customthe filtrate evaporated
  4. dissolutionThe residue is dissolved in ether
  5. washthe solution washed two times with a little cold water
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated

Sources & evidence

ORD record
ord-b6cd323898504e1db19ee8ddc86abeb6
Source dataset
uspto-grants-1982_09
Patent number
US04351838

Reaction notes

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