Potassium Carbonate → HCID 14472333, compound

HRID 345750Notes

Reaction equation

HRID 345750 reaction equation
F[B-](F)(F)F.[CH2:6]([O+](CC)CC)[CH3:7].[CH3:13][C:14]1([CH3:21])[NH:17][C:16](=[O:18])[C:15]1([CH3:20])[CH3:19].C([O-])([O-])=O.[K+].[K+]>ClCCl>[CH2:6]([O:18][C:16]1[C:15]([CH3:20])([CH3:19])[C:14]([CH3:21])([CH3:13])[N:17]=1)[CH3:7]

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 5501512-Azetidinone, 3,3,4,4-tetramethyl-HCID 2723982Triethyloxonium tetrafluoroborate

Product 1

HCID 14472333HCID 14472333, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent3×

Procedure

To a solution of 60 ml (1M) of triethyloxonium tetrafluoroborate in dichloromethane was added 5 g (0.039 mol) of tetramethylazetidinone in 10 ml of dry CH2Cl2 under an inert atmosphere. The reaction mixture was stirred for 1 hour at room temperature and then was refluxed for 1 hour. After cooling, the reaction mixture was added dropwise to 20 ml of a 50% K2CO3 solution at -10° C. and the mixture was diluted with 20 ml of CH2Cl2 and then filtered. The organic phase was separated out and immediately dried over MgSO4. After filtration, the solvent was stripped off under vacuum and the residue was distilled at 78° to 80° C./50 mmHg to obtain the product as a colorless oil.

Workup

  1. temperaturewas refluxed for 1 hour
  2. temperatureAfter cooling
  3. filtrationfiltered
  4. customThe organic phase was separated out
  5. dry with materialimmediately dried over MgSO4
  6. filtrationAfter filtration
  7. distillationthe residue was distilled at 78° to 80° C./50 mmHg

Sources & evidence

ORD record
ord-78c3ad9775be44f9adc75c922ae7cd74
Source dataset
uspto-grants-1991_10
Patent number
US05059596

Reaction notes

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