Sodium Hydroxide → FK 1052
Reaction equation
[CH3:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]2[C:11](=[O:22])[CH:12]([CH2:15][C:16]3[N:17]=[CH:18][NH:19][C:20]=3[CH3:21])[CH2:13][CH2:14][C:3]=12.CC1(C)C2(CS(O)(=O)=O)C(CC1CC2)=O.[OH-].[Na+]>CO.O>[CH3:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]2[C:11](=[O:22])[CH:12]([CH2:15][C:16]3[N:17]=[CH:18][NH:19][C:20]=3[CH3:21])[CH2:13][CH2:14][C:3]=12Participants
5
Reagents, catalysts & solvents 2
Procedure
(+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one·CSA salt (15.0 g) was suspended in methanol (45 ml) and water (105 ml), and adjusted to pH10.6 with 8% aqueous sodium hydroxide (10 ml) at an interior temperature of 20~30° C. It was agitated for 1 hr at the same temperature, thereafter the crystals were collected by filtration, washed with water (45 ml), and thereafter dried overnight under vacuum to obtain (+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one.
Workup
- filtrationthe crystals were collected by filtration
- washwashed with water (45 ml)
- customdried overnight under vacuum
Sources & evidence
- ORD record
- ord-160367fd4b704c67b8ebcacca7ea1b64
- Source dataset
- uspto-grants-2000_01
- Patent number
- US06013653
Reaction notes
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