Hydrochloric Acid → 6-{6-[2-(1-ethylpiperidin-4-yl)ethoxy]-5-(trifluoromethyl)pyridin-3-yl}-9-methyl-9H-purine-2-carbonitrile monohydrochloride

HRID 522304노트

반응식

HRID 522304 반응식
[ClH:1].[CH2:2]([N:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][O:12][C:13]2[N:18]=[CH:17][C:16]([C:19]3[N:27]=[C:26]([C:28]#[N:29])[N:25]=[C:24]4[C:20]=3[N:21]=[CH:22][N:23]4[CH3:30])=[CH:15][C:14]=2[C:31]([F:34])([F:33])[F:32])[CH2:6][CH2:5]1)[CH3:3]>CCOC(C)=O.CCO>[ClH:1].[CH2:2]([N:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][O:12][C:13]2[N:18]=[CH:17][C:16]([C:19]3[N:27]=[C:26]([C:28]#[N:29])[N:25]=[C:24]4[C:20]=3[N:21]=[CH:22][N:23]4[CH3:30])=[CH:15][C:14]=2[C:31]([F:33])([F:32])[F:34])[CH2:6][CH2:5]1)[CH3:3]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 717616296-{6-[2-(1-ethylpiperidin-4-yl)ethoxy]-5-(trifluoromethyl)pyridin-3-yl}-9-methyl-9H-purine-2-carbonitrile

생성물 1

HCID 1178995926-{6-[2-(1-ethylpiperidin-4-yl)ethoxy]-5-(trifluoromethyl)pyridin-3-yl}-9-methyl-9H-purine-2-carbonitrile monohydrochloride

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

A 4 M solution of hydrogen chloride in EtOAc (4.2 mL) was added dropwise to a suspension of 6-{6-[2-(1-ethylpiperidin-4-yl)ethoxy]-5-(trifluoromethyl)pyridin-3-yl}-9-methyl-9H-purine-2-carbonitrile (3.9 g) in EtOH (58.5 mL) at room temperature, whereby a solution was obtained. After the solution was concentrated under reduced pressure, the residue was suspended in EtOH (117 mL). The suspension was stirred at 80° C. to obtain a solution, and the solution was cooled to room temperature while stirring. The solution was stirred at room temperature overnight. The precipitated solid was filtered, and the solid was washed with EtOH, whereby 6-{6-[2-(1-ethylpiperidin-4-yl)ethoxy]-5-(trifluoromethyl)pyridin-3-yl}-9-methyl-9H-purine-2-carbonitrile monohydrochloride (3.2 g) was obtained as a crystal (heat absorption peak temperature obtained by a TG/DTA analysis: near 220° C.).

후처리

  1. customwhereby a solution was obtained
  2. concentrationAfter the solution was concentrated under reduced pressure
  3. customto obtain a solution
  4. temperaturethe solution was cooled to room temperature
  5. stirringwhile stirring
  6. stirringThe solution was stirred at room temperature overnight
  7. filtrationThe precipitated solid was filtered
  8. washthe solid was washed with EtOH

출처 및 근거

ORD 기록
ord-396c0dad0d3b4c239aa9998bf3acf0f1
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09328118B2

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