Reaction equation
[CH3:1][C:2]1[CH:10]=[C:9]([C:11]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]3[C:29]4[C:24](=[CH:25][C:26]([O:32][CH3:33])=[C:27]([O:30][CH3:31])[CH:28]=4)[N:23]=[C:22]([NH:34][CH3:35])[N:21]=3)[CH:15]=2)=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]>O1CCCC1>[OH2:5].[CH3:1][C:2]1[CH:10]=[C:9]([C:11]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]3[C:29]4[C:24](=[CH:25][C:26]([O:32][CH3:33])=[C:27]([O:30][CH3:31])[CH:28]=4)[N:23]=[C:22]([NH:34][CH3:35])[N:21]=3)[CH:15]=2)=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]Participants
Procedure
The third crystals of methyl N-[3-(6,7-dimethoxy-2-methylaminoquinazolin-4-yl)phenyl]terephthalamic acid hydrate can be produced by dissolving methyl N-[3-(6,7-dimethoxy-2-methylaminoquinazolin-4-yl)phenyl]terephthalamic acid in tetrahydrofuran and precipitating crystals from the solution. More particularly, the third crystals of methyl N-[3-(6,7-dimethoxy-2-methylaminoquinazolin-4-yl)phenyl]terephthalamic acid hydrate can be produced by dissolving methyl N-[3-(6,7-dimethoxy-2-methylaminoquinazolin-4-yl)phenyl]terephthalamic acid in tetrahydrofuran at room temperature or under heating and slowly cooling the solution to 4° C. to room temperature to precipitate crystals from the solution. Upon crystallization, water can be added. The amount of tetrahydrofuran used can be appropriately selected, provided that the lower limit is the amount that enables the dissolution of methyl N-[3-(6,7-dimethoxy-2-methylaminoquinazolin-4-yl)phenyl]terephthalamic acid by heating and the upper limit is the amount that does not decrease the yield of the crystals significantly.
Workup
- customprecipitating crystals from the solution
Sources & evidence
- ORD record
- ord-60284781e4124a9eae4557581994e8a4
- Source dataset
- uspto-grants-2013_09
- Patent number
- US08530654B2
Linked notes
Loading…