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 1926136ノート

反応式

HRID 1926136 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][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

参加物

4

反応物 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

生成物 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)収率 76.9%

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}-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.

後処理

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

出典と根拠

ORDレコード
ord-6e899469724a483ead3b7a3c9e49a8bf
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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