1-Propanesulfonic acid → 3-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}-phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester propanesulfonate

HRID 2089696

Reaktionsgleichung

Reaktionsgleichung von HRID 2089696
[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:9]([F:56])=[C:10]([C@@H:16]([NH:39][C:40]2[CH:45]=[CH:44][C:43]([C:46]([NH2:55])=[N:47][C:48]([O:50][CH2:51][C:52]([CH3:54])=[CH2:53])=[O:49])=[CH:42][CH:41]=2)[C:17]2[N:18]=[C:19]([O:28][CH2:29][O:30][C:31](=[O:38])[C:32]([CH3:37])([CH3:36])[CH2:33][O:34][CH3:35])[N:20]([C:22]3[N:27]=[CH:26][CH:25]=[CH:24][N:23]=3)[N:21]=2)[CH:11]=[C:12]([O:14][CH3:15])[CH:13]=1)(=[O:3])[CH3:2].[CH2:57]([S:60]([OH:63])(=[O:62])=[O:61])[CH2:58][CH3:59]>C(OCC)(=O)C>[CH2:57]([S:60]([OH:63])(=[O:62])=[O:61])[CH2:58][CH3:59].[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:9]([F:56])=[C:10]([C@@H:16]([NH:39][C:40]2[CH:41]=[CH:42][C:43]([C:46]([NH2:55])=[N:47][C:48]([O:50][CH2:51][C:52]([CH3:54])=[CH2:53])=[O:49])=[CH:44][CH:45]=2)[C:17]2[N:18]=[C:19]([O:28][CH2:29][O:30][C:31](=[O:38])[C:32]([CH3:37])([CH3:36])[CH2:33][O:34][CH3:35])[N:20]([C:22]3[N:27]=[CH:26][CH:25]=[CH:24][N:23]=3)[N:21]=2)[CH:11]=[C:12]([O:14][CH3:15])[CH:13]=1)(=[O:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 789381-Propanesulfonic acidHCID 674711843-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester

Produkt 1

HCID 866774063-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}-phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester propanesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

At room temperature, 3-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester (1.0 g, 1.28 mmol) was dissolved in ethyl acetate (100 mL), a solution of 1-propanesulfonic acid [CAS No. 5284-66-2] (151 mg, 1.22 mmol) in ethyl acetate (5 mL) was added dropwise thereto. To the resulting mixture, a seed crystal of the captioned compound was added, and the resulting mixture was stirred overnight at room temperature. The precipitated solid was filtered, sequentially washed with ethyl acetate and tert-butyl methyl ether, and then dried to obtain the captioned compound (950 mg) as a white powder.

Aufarbeitung

  1. additionTo the resulting mixture, a seed crystal of the captioned compound was added
  2. filtrationThe precipitated solid was filtered
  3. washsequentially washed with ethyl acetate and tert-butyl methyl ether
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-ea1de7d801834d919e3cabdf8bfd1a2c
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08436009B2

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