p-Toluenesulfonic acid → 4-(1H-Imidazol-1-yl)-2-(6-piperidin-1-ylpyrimidin-4-yl)-1,2-dihydro-3H-pyrazol-3-one

HRID 876689ノート

反応式

HRID 876689 の反応式
C(O[C:4](=[O:15])[C:5]([N:10]1[CH:14]=[CH:13][N:12]=[CH:11]1)=[CH:6][N:7](C)C)C.[NH:16]([C:18]1[CH:23]=[C:22]([N:24]2[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]2)[N:21]=[CH:20][N:19]=1)N.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(OCC)(=O)C>[N:10]1([C:5]2[C:4](=[O:15])[N:16]([C:18]3[CH:23]=[C:22]([N:24]4[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29]4)[N:21]=[CH:20][N:19]=3)[NH:7][CH:6]=2)[CH:14]=[CH:13][N:12]=[CH:11]1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 441403054-Hydrazinyl-6-(piperidin-1-yl)pyrimidineHCID 66726242Ethyl 3-(N,N-dimethylamino)-2-(1H-imidazol-1-yl)acrylate

生成物 1

HCID 596036554-(1H-Imidazol-1-yl)-2-(6-piperidin-1-ylpyrimidin-4-yl)-1,2-dihydro-3H-pyrazol-3-one

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

5.5 g (26.3 mmol) of the compound from Example 42A and 6.1 g (31.5 mmol) of the compound from Example 8A are dissolved in 55 ml ethyl acetate and 1.2 g (10.5 mmol) p-toluenesulfonic acid are added. The mixture is heated to the reflux and is stirred at this temperature for 16 h. After cooling to RT, the precipitate is filtered off and washed with ethyl acetate. The solid is dissolved in 50 ml water and the solution is adjusted to pH 7 with 1 N hydrochloric acid. The precipitate is filtered off, washed with water and diisopropyl ether and finally dried over phosphorus pentoxide.

後処理

  1. temperatureThe mixture is heated to the
  2. temperaturereflux
  3. filtrationthe precipitate is filtered off
  4. washwashed with ethyl acetate
  5. dissolutionThe solid is dissolved in 50 ml water
  6. filtrationThe precipitate is filtered off
  7. washwashed with water and diisopropyl ether
  8. dry with materialfinally dried over phosphorus pentoxide

出典と根拠

ORDレコード
ord-91fe875019474c7ca477ef0141dff174
出典データセット
uspto-grants-2015_03
特許番号
US08987261B2

反応ノート

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