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

HRID 522304ノート

反応式

HRID 522304 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-396c0dad0d3b4c239aa9998bf3acf0f1
出典データセット
uspto-grants-2016_05
特許番号
US09328118B2

反応ノート

読み込み中…