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

HRID 1942023노트

반응식

HRID 1942023 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-93bce623449f4ff5bc5dae95572aa2a3
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389520B2

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