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Hydrochloric Acid → (3r)-n-[(3-{[3-{[(5-Chloro-2-thienyl)sulfonyl]amino}-4-(1-hydroxy-1-methylethyl)-1h-indazol-1-yl]methyl}phenyl)methyl]-3-morpholinecarboxamide formate salt

HRID 1808645
ノート
印刷プレビュー

反応式

HRID 1808645 の反応式
CCN(C(C)C)C(C)C.CC([O:14][C:15]([N:17]1[CH2:22][CH2:21][O:20][CH2:19][C@@H:18]1[C:23]([OH:25])=O)=[O:16])(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:50][CH2:51][C:52]1[CH:53]=[C:54]([CH2:58][N:59]2[C:67]3[C:62](=[C:63]([C:68]([OH:71])([CH3:70])[CH3:69])[CH:64]=[CH:65][CH:66]=3)[C:61]([NH:72][S:73]([C:76]3[S:77][C:78]([Cl:81])=[CH:79][CH:80]=3)(=[O:75])=[O:74])=[N:60]2)[CH:55]=[CH:56][CH:57]=1.Cl.O1CCOCC1>C(Cl)Cl.CO>[CH:15]([OH:16])=[O:14].[Cl:81][C:78]1[S:77][C:76]([S:73]([NH:72][C:61]2[C:62]3[C:67](=[CH:66][CH:65]=[CH:64][C:63]=3[C:68]([OH:71])([CH3:69])[CH3:70])[N:59]([CH2:58][C:54]3[CH:53]=[C:52]([CH2:51][NH:50][C:23]([C@H:18]4[CH2:19][O:20][CH2:21][CH2:22][NH:17]4)=[O:25])[CH:57]=[CH:56][CH:55]=3)[N:60]=2)(=[O:74])=[O:75])=[CH:80][CH:79]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 81531DiisopropylethylamineHCID 1512538(3R)-4-(tert-Butoxycarbonyl)morpholine-3-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 59456043
N-[1-{[3-(Aminomethyl)phenyl]methyl}-4-(1-hydroxy-1-methylethyl)-1H-indazol-3-yl]-5-chloro-2-thiophenesulfonamide

生成物 1

HCID 66664136(3r)-n-[(3-{[3-{[(5-Chloro-2-thienyl)sulfonyl]amino}-4-(1-hydroxy-1-methylethyl)-1h-indazol-1-yl]methyl}phenyl)methyl]-3-morpholinecarboxamide formate salt収率 5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

DIPEA (0.057 mL, 0.326 mmol) was added to a stirring solution of (3R)-4-{[(1,1-dimethylethyl)oxy]carbonyl}-3-morpholinecarboxylic acid (18.84 mg, 0.081 mmol) in DCM (1 mL). HATU (31.0 mg, 0.081 mmol) was then added, followed by N-[1-{[3-(aminomethyl)phenyl]methyl}-4-(1-hydroxy-1-methylethyl)-1H-indazol-3-yl]-5-chloro-2-thiophenesulfonamide (for a preparation see Intermediate 78) (40 mg, 0.081 mmol) and the reaction was stirred for an hour at room temp. The reaction mixture was concentrated and 4N Hydrogen chloride in dioxane (0.020 mL, 0.081 mmol) was then added and the reaction stirred at room temperature for 0.5 h. The reaction mixture was passed through a pre-conditioned (MeOH) SCX-2 cartridge, washed with methanol and then eluted using 2M ammonia in methanol. The appropriate ammoniacal fractions were concentrated, and the residue was dissolved in DMSO (0.5 mL) and purified by Mass Directed AutoPrep on Sunfire C18 column using Acetonitrile Water with a Formic acid modifier (Method A). The solvent was removed under a stream of nitrogen in the Radleys blowdown apparatus to give the title compound (2.7 mg, 5%). LCMS (System F) RT=0.84 min, ES+ve m/z 604/606 (M+H)+.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. stirringthe reaction stirred at room temperature for 0.5 h
  3. washwashed with methanol
  4. washeluted
  5. concentrationThe appropriate ammoniacal fractions were concentrated
  6. dissolutionthe residue was dissolved in DMSO (0.5 mL)
  7. custompurified by Mass Directed AutoPrep on Sunfire C18 column
  8. customThe solvent was removed under a stream of nitrogen in the Radleys blowdown apparatus

出典と根拠

ORDレコード
ord-77b006dee4da4a359dedb7e4bc0c255a
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08357716B2

反応ノート

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