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 1926138노트

반응식

HRID 1926138 반응식
[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

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 11620908Tak-285

생성물 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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-5da901f460e946208cc5a208d7ed3b65
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178543B2

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