HCID 9937786, compound → HCID 86759179, compound
Reaction equation
[OH2:1].[OH2:2].[C:3]1([CH:9]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[O:10][CH:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][CH2:19][NH:20][C:21]3[CH:22]=[CH:23][C:24]4[N:25]([CH:27]=[C:28]([C:30]([CH3:35])([CH3:34])[C:31]([OH:33])=[O:32])[N:29]=4)[N:26]=3)[CH2:13][CH2:12]2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>C(O)C>[C:36]1([CH:9]([C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)[O:10][CH:11]2[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][CH2:19][NH:20][C:21]3[CH:22]=[CH:23][C:24]4[N:25]([CH:27]=[C:28]([C:30]([CH3:35])([CH3:34])[C:31]([O:33][C:34](=[O:2])[C:30]([CH3:35])([C:28]5[N:29]=[C:24]6[CH:23]=[CH:22][C:21]([NH:20][CH2:19][CH2:18][CH2:17][N:14]7[CH2:15][CH2:16][CH:11]([O:1][CH:9]([C:36]8[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=8)[C:3]8[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=8)[CH2:12][CH2:13]7)=[N:26][N:25]6[CH:27]=5)[CH3:31])=[O:32])[N:29]=4)[N:26]=3)[CH2:15][CH2:16]2)[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
In 500 mL of ethanol, 3.20 g (5.67 mmol) of the 2-[6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionic acid dihydrate obtained in Example 135A was dissolved under heating, followed by concentrating at atomospheric pressure until the total volume became 250 mL. After standing at room temperature, the crystals formed were collected by filtration, washed with ethanol and dried to yield 2.67 g of the title compound.
Workup
- temperatureunder heating
- concentrationby concentrating at atomospheric pressure until the total volume
- customAfter standing at room temperature
- customthe crystals formed
- filtrationwere collected by filtration
- washwashed with ethanol
- customdried
Sources & evidence
- ORD record
- ord-95fa5a7e476d49df95001093df57e5dd
- Source dataset
- uspto-grants-2003_09
- Patent number
- US06627630B1
Reaction notes
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