Potassium Carbonate → HCID 21525488, compound
Reaction equation
[CH3:1][C:2]1[CH:16]=[CH:15][C:5]([O:6][CH2:7][CH2:8][N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[C:4]([O:17][CH3:18])[CH:3]=1.[F:19][C:20]1[CH:31]=[CH:30][C:23]([C:24]([CH2:26][CH2:27][CH2:28][Cl:29])=[O:25])=[CH:22][CH:21]=1.C(=O)([O-])[O-].[K+].[K+].[Br-].[K+]>>[ClH:29].[ClH:29].[F:19][C:20]1[CH:21]=[CH:22][C:23]([C:24]([CH2:26][CH2:27][CH2:28][N:12]2[CH2:13][CH2:14][N:9]([CH2:8][CH2:7][O:6][C:5]3[CH:15]=[CH:16][C:2]([CH3:1])=[CH:3][C:4]=3[O:17][CH3:18])[CH2:10][CH2:11]2)=[O:25])=[CH:30][CH:31]=1Participants
Procedure
A mixture of 25.0 grams of 1-[2-(4-methyl-2-methoxyphenoxy)ethyl]piperazine, 20.1 grams of 3-(4-fluorobenzoyl)propyl chloride, 13.8 grams of potassium carbonate and 10 grams of potassium bromide was heated under gentle reflux for a period of 24 hours. The resulting reaction mixture was filtered while hot and the filtrate after cooling was acidified by adding thereto with stirring a 10% solution of hydrochloric acid, whereupon the compound that is specified in the heading separated. The resulting precipitate was then separated by filtration and recrystallized from a mixture of 80 parts by volume of ethanol and 20 parts by volume of water. In this manner, 15 grams of the salt specified in the heading, having a melting point of 211°-213°C, was obtained.
Workup
- temperaturewas heated
- temperatureunder gentle reflux for a period of 24 hours
- customThe resulting reaction mixture
- filtrationwas filtered while hot and the filtrate
- temperatureafter cooling
- additionby adding
- customheading separated
- customThe resulting precipitate was then separated by filtration
- customrecrystallized from a mixture of 80 parts by volume of ethanol and 20 parts by volume of water
- customwas obtained
Sources & evidence
- ORD record
- ord-55d4847d18c640d7ae8266582277c9c9
- Source dataset
- uspto-grants-1976_06
- Patent number
- US03966735
Reaction notes
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