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Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → N-{1-[(4-Oxopiperidin-1-yl)carbonyl]-5-[4-(trifluoromethyl)phenyl]piperidin-3-yl}cyclopentanecarboxamide

HRID 876348
ノート
印刷プレビュー

反応式

HRID 876348 の反応式
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.O1[C:22]2([CH2:27][CH2:26][N:25]([C:28]([N:30]3[CH2:35][CH:34]([C:36]4[CH:41]=[CH:40][C:39]([C:42]([F:45])([F:44])[F:43])=[CH:38][CH:37]=4)[CH2:33][CH:32]([NH:46][C:47]([CH:49]4[CH2:53][CH2:52][CH2:51][CH2:50]4)=[O:48])[CH2:31]3)=[O:29])[CH2:24][CH2:23]2)[O:21]CC1>CC(C)=O.O>[O:21]=[C:22]1[CH2:27][CH2:26][N:25]([C:28]([N:30]2[CH2:35][CH:34]([C:36]3[CH:41]=[CH:40][C:39]([C:42]([F:45])([F:43])[F:44])=[CH:38][CH:37]=3)[CH2:33][CH:32]([NH:46][C:47]([CH:49]3[CH2:53][CH2:52][CH2:51][CH2:50]3)=[O:48])[CH2:31]2)=[O:29])[CH2:24][CH2:23]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)2 回HCID 66701500N-{1-(1,4-Dioxa-8-azaspiro[4.5]dec-8-ylcarbonyl)-5-[4-(trifluoromethyl)phenyl]piperidin-3-yl}-cyclopentanecarboxamide

生成物 1

HCID 46931417N-{1-[(4-Oxopiperidin-1-yl)carbonyl]-5-[4-(trifluoromethyl)phenyl]piperidin-3-yl}cyclopentanecarboxamide

試薬・触媒・溶媒 1

HCID 18366337Propan-2-one--water (1/1)溶媒

実験手順

14.3 mg of pyridinium p-toluenesulphonate (0.057 mmol) were added to a solution of the acetal from Example 63A (97.2 mg, 0.191 mmol) in 5.5 ml of acetone/water (10:1), and the mixture was stirred under reflux overnight. Another 14.3 mg of pyridinium p-toluenesulphonate (0.057 mmol) were added, and the mixture was stirred under reflux for another night. The mixture was then cooled, and the precipitate formed was filtered off. Yield: 66.2 mg (74% of theory)

後処理

  1. temperatureunder reflux overnight
  2. stirringthe mixture was stirred
  3. temperatureunder reflux for another night
  4. temperatureThe mixture was then cooled
  5. customthe precipitate formed
  6. filtrationwas filtered off

出典と根拠

ORDレコード
ord-d68b0c0211f545a48670a6127fbec740
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08987248B2

反応ノート

読み込み中…

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