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 1521461노트

반응식

HRID 1521461 반응식
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

참가 물질

7

반응물 4

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

생성물 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

시약·촉매·용매 2

HCID 6560Isobutanol용매HCID 66787386Toluene iso-butanol용매

실험 절차

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.

후처리

  1. temperatureto cool

출처 및 근거

ORD 기록
ord-ed5fde46edf04fd1932b7de1cb17a256
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073928B2

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