Potassium Carbonate → HCID 59536717, compound

HRID 709131Notes

Reaction equation

HRID 709131 reaction equation
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[C:13]([Cl:14])=[CH:12][CH:11]=[CH:10][C:9]=1[CH:15]([NH:25][C:26](=[O:32])[O:27][C:28]([CH3:31])([CH3:30])[CH3:29])S(C1C=CC=CC=1)(=O)=O>C1COCC1>[Cl:7][C:8]1[C:13]([Cl:14])=[CH:12][CH:11]=[CH:10][C:9]=1/[CH:15]=[N:25]/[C:26](=[O:32])[O:27][C:28]([CH3:30])([CH3:29])[CH3:31]

Participants

4

Procedure

4.42 g (32.0 mmol) of potassium carbonate were dried in the heat under high vacuum and then cooled to RT under an atmosphere of argon. 52 ml of anhydrous THF and 2.22 g (5.33 mmol) of the compound of Example 21A were added. The reaction mixture was then stirred at reflux temperature for 16 h. After cooling to RT, the reaction mixture was filtered through Celite. The solid was washed with a little THF. The combined filtrates were freed from the solvent on a rotary evaporator and the residue was dried under high vacuum. This gave 1.38 g (94% of theory) of the title compound.

Workup

  1. temperatureheat under high vacuum
  2. temperatureat reflux temperature for 16 h
  3. temperatureAfter cooling to RT
  4. filtrationthe reaction mixture was filtered through Celite
  5. washThe solid was washed with a little THF
  6. customThe combined filtrates were freed from the solvent on a rotary evaporator
  7. customthe residue was dried under high vacuum

Sources & evidence

ORD record
ord-49f1f4f08abf4959b27194a41e0603d8
Source dataset
uspto-grants-2015_11
Patent number
US09180120B2

Reaction notes

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