Dichloromethane → 2-Methylene-3-quinuclidone

HRID 745539

Reaction equation

HRID 745539 reaction equation
Cl.O.O.[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2.C(=O)([O-])[O-].[K+].[K+].C(Cl)Cl>O>[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 219542752-Methylene-3-quinuclidinone dihydrate hydrochloride

Product 1

HCID 3229732-Methylene-3-quinuclidone

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Suspend 95.4 g (0.455 mole) 2-methylene-3-quinuclidinone dihydrate hydrochloride in a solution of 255 g (1.85 moles) anhydrous potassium carbonate dissolved in 350 ml H2O. When the suspension clears add 500 ml methylene chloride and mix the 2-phase system overnight using a mechanical stirrer. Separate the layers and dry the methylene chloride layer over potassium carbonate. Remove the solvents in vacuo to obtain the title compound. Repeat the extraction until most of the product is collected.

Workup

  1. additionmix the 2-phase system overnight
  2. customSeparate the layers
  3. dry with materialdry the methylene chloride layer over potassium carbonate
  4. customRemove the solvents in vacuo

Sources & evidence

ORD record
ord-8487bf1433834c318e8cfa3a4af4c32e
Source dataset
uspto-grants-1986_07
Patent number
US04599344

Linked notes

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