Hydrochloric Acid → 3-{3-[3-({[(2,2,2-Trifluoroethyl)amino]carbonyl}amino)phenyl]imidazo[1,2-b]pyridazin-7-yl}benzoic acid

HRID 407079ノート

反応式

HRID 407079 の反応式
O.[OH-].[Li+].[F:4][C:5]([F:37])([F:36])[CH2:6][NH:7][C:8]([NH:10][C:11]1[CH:12]=[C:13]([C:17]2[N:21]3[N:22]=[CH:23][C:24]([C:26]4[CH:27]=[C:28]([CH:33]=[CH:34][CH:35]=4)[C:29]([O:31]C)=[O:30])=[CH:25][C:20]3=[N:19][CH:18]=2)[CH:14]=[CH:15][CH:16]=1)=[O:9].C1COCC1.Cl>CO.O>[F:37][C:5]([F:4])([F:36])[CH2:6][NH:7][C:8]([NH:10][C:11]1[CH:12]=[C:13]([C:17]2[N:21]3[N:22]=[CH:23][C:24]([C:26]4[CH:27]=[C:28]([CH:33]=[CH:34][CH:35]=4)[C:29]([OH:31])=[O:30])=[CH:25][C:20]3=[N:19][CH:18]=2)[CH:14]=[CH:15][CH:16]=1)=[O:9]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 67980357Methyl 3-{3-[3-({[(2,2,2-trifluoro ethyl)amino]carbonyl}amino)phenyl]imidazo[1,2-b]pyridazin-7-yl}benzoate

生成物 1

HCID 679803273-{3-[3-({[(2,2,2-Trifluoroethyl)amino]carbonyl}amino)phenyl]imidazo[1,2-b]pyridazin-7-yl}benzoic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Lithium hydroxide monohydrate (40. mg, 0.96 mmol) was added to a mixture of methyl 3-{3-[3-({[(2,2,2-trifluoro ethyl)amino]carbonyl}amino)phenyl]imidazo[1,2-b]pyridazin-7-yl}benzoate (0.090 g, 0.19 mmol) in methanol (2.0 mL)/THF (1.0 mL)/water (0.5 mL) and then the reaction was stirred at r.t. for 4 h. The mixture was adjusted with conc. HCl to PH˜3, and then concentrated under reduced pressure to give the crude product which was directly used in the next reaction without further purification. LCMS (M+H)+: m/z=456.1

後処理

  1. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f8b6612c293748238c389b75829d47b1
出典データセット
uspto-grants-2014_06
特許番号
US08754114B2

反応ノート

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