Methanesulfonic Acid → N-{2-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-3-hydroxy-3-methylbutanamide methanesulfonate

HRID 1926138ノート

反応式

HRID 1926138 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:19][C:20]2[C:21]3[N:28]([CH2:29][CH2:30][NH:31][C:32](=[O:38])[CH2:33][C:34]([OH:37])([CH3:36])[CH3:35])[CH:27]=[CH:26][C:22]=3[N:23]=[CH:24][N:25]=2)[CH:5]=[CH:6][C:7]=1[O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=1.[CH3:39][S:40]([OH:43])(=[O:42])=[O:41]>C(OCC)(=O)C>[CH3:39][S:40]([OH:43])(=[O:42])=[O:41].[Cl:1][C:2]1[CH:3]=[C:4]([NH:19][C:20]2[C:21]3[N:28]([CH2:29][CH2:30][NH:31][C:32](=[O:38])[CH2:33][C:34]([OH:37])([CH3:35])[CH3:36])[CH:27]=[CH:26][C:22]=3[N:23]=[CH:24][N:25]=2)[CH:5]=[CH:6][C:7]=1[O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=1

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 11620908Tak-285

生成物 1

HCID 86615788N-{2-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-3-hydroxy-3-methylbutanamide methanesulfonate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of N-{2-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-3-hydroxy-3-methylbutanamide (200 mg) in ethyl acetate (10 mL) was added methanesulfonic acid (26 μL) at room temperature. The mixture was stirred at room temperature for 1 hr and concentrated under reduced pressure. To the residue were added ethanol and ethyl acetate, and the precipitated crystals were collected by filtration to give the title compound (223 mg) as colorless crystals.

後処理

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue were added ethanol and ethyl acetate
  3. filtrationthe precipitated crystals were collected by filtration

出典と根拠

ORDレコード
ord-5da901f460e946208cc5a208d7ed3b65
出典データセット
uspto-grants-2012_05
特許番号
US08178543B2

反応ノート

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