Hydrogen Bromide → Formate

HRID 40297

反応式

HRID 40297 の反応式
Cl.[CH3:2][O:3][C:4]1[CH:13]=[C:12]2[C:7]([C:8]([NH:14][CH2:15][C:16]3[N:20]4[N:21]=[C:22]([C:25]5[CH:30]=[C:29]([F:31])[C:28]([F:32])=[C:27]([F:33])[CH:26]=5)[CH:23]=[CH:24][C:19]4=[N:18][N:17]=3)=[CH:9][CH:10]=[N:11]2)=[N:6][CH:5]=1.Br.[OH-:35].[Na+]>>[F:33][C:27]1[CH:26]=[C:25]([C:22]2[CH:23]=[CH:24][C:19]3[N:20]([C:16]([CH2:15][NH:14][C:8]4[CH:9]=[CH:10][N:11]=[C:12]5[C:7]=4[N:6]=[CH:5][C:4]([OH:3])=[CH:13]5)=[N:17][N:18]=3)[N:21]=2)[CH:30]=[C:29]([F:31])[C:28]=1[F:32].[CH:2]([O-:3])=[O:35]

参加物

5

反応物 3

HCID 260Hydrogen BromideHCID 14798Sodium HydroxideHCID 675036137-methoxy-N-((6-(3,4,5-trifluorophenyl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methyl)-1,5-naphthyridin-4-amine hydrochloride

生成物 2

HCID 283FormateHCID 1359874698-((6-(3,4,5-Trifluorophenyl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylamino)-1,5-naphthyridin-3-ol

実験手順

A sealed tube was charged with 7-methoxy-N-((6-(3,4,5-trifluorophenyl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methyl)-1,5-naphthyridin-4-amine hydrochloride (238 mg, 502 μmol) and HBr (5966 μl, 52740 μmol), sealed, then placed in a 120° C. oil bath for 48 h. Cooled to room temperature and brought to pH˜14 with NaOH (6N). Isolated solid by filtration which was purified by RPHPLC to afford 8-((6-(3,4,5-trifluorophenyl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylamino)-1,5-naphthyridin-3-ol as its formate salt. MS (ESI pos. ion) m/z: 424 (MH+). Calc'd exact mass for C20H12F3N2O: 423.

後処理

  1. customsealed
  2. customplaced in a 120° C.
  3. customfor 48 h
  4. customIsolated solid
  5. filtrationby filtration which
  6. customwas purified by RPHPLC

出典と根拠

ORDレコード
ord-7196d7dea5d042b1a64b07539a7fe5fe
出典データセット
uspto-grants-2013_09
特許番号
US08524900B2

関連ノート

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