1,4-Butane sultone → HCID 19700575, compound
Reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([N:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)=[CH:4][CH:3]=1.[CH2:21]1[CH2:28][O:27][S:24](=[O:26])(=[O:25])[CH2:23][CH2:22]1>C(C(C)=O)C(C)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[N:15]2[CH2:16][CH2:17][N:18]([CH2:28][CH2:21][CH2:22][CH2:23][S:24]([OH:27])(=[O:26])=[O:25])[CH2:19][CH2:20]2)=[CH:4][CH:3]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
After a mixture of [4-fluorophenyl-(2-pyridyl)methyl]piperazine (2.71 g), 1,4-butanesultone (4.08 g) and isobutylmethylketone (60 ml) is heated at reflux temperature for 20 hours, precipitated crystals are collected by filtration and recrystallized from ethanol-acetone to give the title compound (2.91 g, 71.5%). mp. 231°-232° C.
Workup
- temperatureis heated
- temperatureat reflux temperature for 20 hours
- customprecipitated crystals
- filtrationare collected by filtration
- customrecrystallized from ethanol-acetone
Sources & evidence
- ORD record
- ord-8261f78e0e6f4ebbbbc5e273982b29bf
- Source dataset
- uspto-grants-1998_02
- Patent number
- US05716950
Reaction notes
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