methyl N-[3-(6,7-dimethoxy-2-methylaminoquinazolin-4-yl)phenyl]terephthalamic acid → methyl N-[3-(6,7-dimethoxy-2-methylaminoquinazolin-4-yl)phenyl]terephthalamic acid hydrate

HRID 41487

반응식

HRID 41487 반응식
[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]

참가 물질

3

실험 절차

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.

후처리

  1. customprecipitating crystals from the solution

출처 및 근거

ORD 기록
ord-60284781e4124a9eae4557581994e8a4
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530654B2

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