Potassium Carbonate → HCID 17842074, compound

HRID 645338Notes

Reaction equation

HRID 645338 reaction equation
[CH:1]1([C:5]([C:7]2[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=2)=O)[CH2:4][CH2:3][CH2:2]1.O.NN.C([O-])([O-])=O.[K+].[K+]>C(O)COCCO>[CH:1]1([CH2:5][C:7]2[CH:8]=[CH:9][C:10]([O:13][CH3:14])=[CH:11][CH:12]=2)[CH2:2][CH2:3][CH2:4]1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 24654Hydrazine hydrate (1:1)HCID 13813654Cyclobutyl(4-methoxyphenyl)methanone

Product 1

HCID 17842074HCID 17842074, compoundYield 95%

Reagents, catalysts & solvents 1

HCID 8117Diethylene GlycolSolvent

Procedure

A mixture of compound (G) (5.00 g), hydrazine hydrate (4.12 g), K2CO3 (7.00 g) and diethylene glycol (16 ml) were heated to reflux temperature for 1 hour. The condenser was exchanged by a distillation device and the mixture was distilled at 220-230° C. The distillate was extracted with MTBE and the organic phase washed with water and brine, dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography to yield a colorless oil (4.4 g).

Workup

  1. temperaturewere heated
  2. temperatureto reflux temperature for 1 hour
  3. distillationthe mixture was distilled at 220-230° C
  4. extractionThe distillate was extracted with MTBE
  5. washthe organic phase washed with water and brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by chromatography

Sources & evidence

ORD record
ord-5303ce8b359346df922f13f96f7808d8
Source dataset
uspto-grants-2010_04
Patent number
US07704942B2

Reaction notes

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