Potassium Carbonate → Aripiprazole

HRID 922167ノート

反応式

HRID 922167 の反応式
C(=O)([O-])[O-].[K+].[K+].Cl[CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:22]=[C:21]2[C:16]([CH2:17][CH2:18][C:19](=[O:23])[NH:20]2)=[CH:15][CH:14]=1.Cl.[Cl:25][C:26]1[C:31]([Cl:32])=[CH:30][CH:29]=[CH:28][C:27]=1[N:33]1[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]1>O>[CH:29]1[CH:28]=[C:27]([N:33]2[CH2:38][CH2:37][N:36]([CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]3[CH:14]=[CH:15][C:16]4[CH2:17][CH2:18][C:19](=[O:23])[NH:20][C:21]=4[CH:22]=3)[CH2:35][CH2:34]2)[C:26]([Cl:25])=[C:31]([Cl:32])[CH:30]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 104674677-(4-Chlorobutoxy)-1,2,3,4-tetrahydroquinolin-2-oneHCID 116303721-(2,3-Dichlorophenyl)piperazine hydrochloride

生成物 1

HCID 60795Aripiprazole収率 75.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Potassium carbonate (8.39 g) was dissolved in water (140 mL), followed by the addition of 7-(4-chlorobutoxy)-3,4-dihydrocarbostyril (19.4 g) and 1-(2,3-dichlorophenyl)piperazine monohydrochloride (16.2 g) thereto. The mixture was refluxed under stirring for about 3 hours. After reaction, the resulting mixture was cooled, and precipitated crystals were filtered. The crystals were dissolved in ethyl acetate (350 mL), and about 210 mL of water/ethyl acetate azeotrope was distilled under reflux. The remaining solution was cooled, and precipitated crystals were filtered. The thus-obtained crystals were dried at 60° C. for 14 hours, thereby obtaining 20.4 g of crude aripiprazole (yield: 74.2%).

後処理

  1. temperatureThe mixture was refluxed
  2. customAfter reaction
  3. temperaturethe resulting mixture was cooled
  4. customprecipitated crystals
  5. filtrationwere filtered
  6. dissolutionThe crystals were dissolved in ethyl acetate (350 mL)
  7. distillationabout 210 mL of water/ethyl acetate azeotrope was distilled
  8. temperatureunder reflux
  9. temperatureThe remaining solution was cooled
  10. customprecipitated crystals
  11. filtrationwere filtered
  12. customThe thus-obtained crystals were dried at 60° C. for 14 hours

出典と根拠

ORDレコード
ord-947a69e652f144cfabd426ecae67b4fd
出典データセット
uspto-grants-2016_03
特許番号
US09278934B2

反応ノート

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