Acetic Anhydride → HCID 19023506, compound
Reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH:17][S:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[NH2:27])(=[O:20])=[O:19])[CH2:9][CH2:8]1.[C:28](OC(=O)C)(=[O:30])[CH3:29]>>[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:8][CH2:9][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH:17][S:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[NH:27][C:28](=[O:30])[CH3:29])(=[O:20])=[O:19])[CH2:11][CH2:12]1Participants
3
Procedure
0.02 mol of N-(4-(4-(2-pyrimidinyl)-1-piperazinyl)butyl)-2-aminobenzenesulphonamide and 0.5 mol of acetic anhydride are stirred at room temperature for 2 hours. The mixture is evaporated to dryness, concentrated aqueous ammonia solution is poured onto the residue and the base is extracted by shaking with methylene chloride. Purification is carried out by chromatography on silica gel; the eluting agent is CH2Cl2 /CH3OH (9:1). The substance is recrystallised from isopropanol.
Workup
- customThe mixture is evaporated to dryness, concentrated aqueous ammonia solution
- additionis poured onto the residue
- extractionthe base is extracted
- customPurification
- customThe substance is recrystallised from isopropanol
Sources & evidence
- ORD record
- ord-37f93c46279f43aaa9f3e9bfddcfc03e
- Source dataset
- uspto-grants-1993_02
- Patent number
- US05187276
Reaction notes
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