Hydrochloric Acid → HCID 22727218, compound
Reaction equation
[Br:1][C:2]1[CH:34]=[CH:33][C:5]2[CH:6]=[C:7]([S:10]([N:13]3[CH2:18][CH2:17][N:16]([NH:19][CH:20]4[CH2:25][CH2:24][N:23]([C:26]5[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=5)[CH2:22][CH2:21]4)[C:15](=[O:32])[CH2:14]3)(=[O:12])=[O:11])[CH2:8][O:9][C:4]=2[CH:3]=1.[ClH:35]>CO.C(OCC)(=O)C>[ClH:35].[ClH:35].[Br:1][C:2]1[CH:34]=[CH:33][C:5]2[CH:6]=[C:7]([S:10]([N:13]3[CH2:18][CH2:17][N:16]([NH:19][CH:20]4[CH2:25][CH2:24][N:23]([C:26]5[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=5)[CH2:22][CH2:21]4)[C:15](=[O:32])[CH2:14]3)(=[O:11])=[O:12])[CH2:8][O:9][C:4]=2[CH:3]=1Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
A suspension of 4-(7-bromo-2H-benzopyran-3-sulfonyl)-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone (600 mg) in methanol (20 ml) was combined with a 4N solution of hydrochloric acid in ethyl acetate (1 ml) to effect a dissolution and the solution was then concentrated. The residue was crystallized from a mixture of ethanol and ethyl acetate, filtered and dried to obtain the title compound (596 mg) as a colorless solid.
Workup
- dissolutiona dissolution
- concentrationthe solution was then concentrated
- customThe residue was crystallized from a mixture of ethanol and ethyl acetate
- filtrationfiltered
- customdried
Sources & evidence
- ORD record
- ord-81d15e387eb44b9c88ce5e37f3982605
- Source dataset
- uspto-grants-2004_04
- Patent number
- US06723722B1
Reaction notes
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