p-Toluenesulfonic acid monohydrate → Acetamide,n-[2-[4-[[3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl]amino]-5h-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl]-2-(methylsulfonyl)-,mono(4-methylbenzenesulfonate)

HRID 1787049노트

반응식

HRID 1787049 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][S:34]([CH3:37])(=[O:36])=[O: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.O.[CH3:40][C:41]1[CH:46]=[CH:45][C:44]([S:47]([OH:50])(=[O:49])=[O:48])=[CH:43][CH:42]=1>C(OCC)(=O)C>[CH3:40][C:41]1[CH:42]=[CH:43][C:44]([S:47]([OH:50])(=[O:49])=[O:48])=[CH:45][CH:46]=1.[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][S:34]([CH3:37])(=[O:36])=[O: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:17])([F:18])[F:16])[CH:10]=1

참가 물질

4

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 57597166N-{2-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-2-(methylsulfonyl)acetamide

생성물 1

HCID 76852991Acetamide,n-[2-[4-[[3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl]amino]-5h-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl]-2-(methylsulfonyl)-,mono(4-methylbenzenesulfonate)수율 76.9%

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}-2-(methylsulfonyl)acetamide (150 mg) in ethyl acetate (10 mL) was added 4-methylbenzenesulfonic acid monohydrate (55.4 mg) at room temperature. The mixture was stirred at room temperature for 20 hrs, and the solvent was evaporated under reduced pressure. The precipitated crystals were collected by filtration and washed with ethyl acetate and diisopropyl ether to give the title compound (150.3 mg) as colorless crystals.

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. filtrationThe precipitated crystals were collected by filtration
  3. washwashed with ethyl acetate and diisopropyl ether

출처 및 근거

ORD 기록
ord-65461c604e27486ea7313b751fc8862c
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07507740B2

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