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 1521461ノート

反応式

HRID 1521461 の反応式
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

参加物

7

反応物 4

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

生成物 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

試薬・触媒・溶媒 2

HCID 6560Isobutanol溶媒HCID 66787386Toluene iso-butanol溶媒

実験手順

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.

後処理

  1. temperatureto cool

出典と根拠

ORDレコード
ord-ed5fde46edf04fd1932b7de1cb17a256
出典データセット
uspto-grants-2015_07
特許番号
US09073928B2

反応ノート

読み込み中…