Acetonitrile → Cyclopropanecarboxamide, N-((4-((8-chloro-4,10-dihydro-1-methylpyrazolo(3,4-b)(1,5)benzodiazepin-5(1H)-yl)carbonyl)-2-fluorophenyl)methyl)-, 4-methylbenzenesulfonate

HRID 1521461Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1521461
O.[C:2]1([CH3:12])[CH:7]=[CH:6][C:5]([S:8]([OH:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[Cl:13][C:14]1[CH:15]=[CH:16][C:17]2[N:26]([C:27]([C:29]3[CH:41]=[CH:40][C:32]([CH2:33][NH:34][C:35]([CH:37]4[CH2:39][CH2:38]4)=[O:36])=[C:31]([F:42])[CH:30]=3)=[O:28])[CH2:25][C:24]3[CH:23]=[N:22][N:21]([CH3:43])[C:20]=3[NH:19][C:18]=2[CH:44]=1.C(#N)C.C(OCC)(=O)C>C(O)C(C)C.C1(C)C=CC=CC=1.C(O)C(C)C>[C:2]1([CH3:12])[CH:3]=[CH:4][C:5]([S:8]([OH:11])(=[O:9])=[O:10])=[CH:6][CH:7]=1.[Cl:13][C:14]1[CH:15]=[CH:16][C:17]2[N:26]([C:27]([C:29]3[CH:41]=[CH:40][C:32]([CH2:33][NH:34][C:35]([CH:37]4[CH2:38][CH2:39]4)=[O:36])=[C:31]([F:42])[CH:30]=3)=[O:28])[CH2:25][C:24]3[CH:23]=[N:22][N:21]([CH3:43])[C:20]=3[NH:19][C:18]=2[CH:44]=1

Komponenten

7

Edukt 4

HCID 6342AcetonitrileHCID 8857Ethyl AcetateHCID 521998p-Toluenesulfonic acid monohydrateHCID 135564707VA-111913

Produkt 1

HCID 135565015Cyclopropanecarboxamide, N-((4-((8-chloro-4,10-dihydro-1-methylpyrazolo(3,4-b)(1,5)benzodiazepin-5(1H)-yl)carbonyl)-2-fluorophenyl)methyl)-, 4-methylbenzenesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6560IsobutanolLösungsmittelHCID 66787386Toluene iso-butanolLösungsmittel

Versuchsvorschrift

A solution of para-toluenesulfonic acid monohydrate in iso-butanol was added to a solution of cyclopropanecarboxylic acid 4-(6-chloro-3-methyl-4,10-dihydro-3H-2,3,4,9-tetraazabenzo[f]azulene-9-carbonyl)-2-fluoro-benzylamide in toluene/iso-butanol. Acetonitrile and ethyl acetate were added. The solution was allowed to cool and seeded with crystals of the title compound (as prepared herein above). After further cooling and stirring, the product was isolated by filtration, washed with ethyl acetate and then dried.

Aufarbeitung

  1. temperatureto cool

Quellen und Nachweise

ORD-Eintrag
ord-ed5fde46edf04fd1932b7de1cb17a256
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09073928B2

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