Water → 7-{4-[4-(2,3-dichlorophenyl)piperazin-1-yl]butoxy}-1,2,3,4-tetrahydroquinolin-2-one hydrate

HRID 2170285ノート

反応式

HRID 2170285 の反応式
[CH:1]1[CH:2]=[C:3]([N:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:21]=[CH:22][C:23]4[CH2:30][CH2:29][C:27](=[O:28])[NH:26][C:24]=4[CH:25]=3)[CH2:11][CH2:10]2)[C:4]([Cl:8])=[C:5]([Cl:7])[CH:6]=1.[OH2:31]>C(O)C>[CH2:30]1[C:23]2[CH:22]=[CH:21][C:20]([O:19][CH2:18][CH2:17][CH2:16][CH2:15][N:12]3[CH2:11][CH2:10][N:9]([C:3]4[CH:2]=[CH:1][CH:6]=[C:5]([Cl:7])[C:4]=4[Cl:8])[CH2:14][CH2:13]3)=[CH:25][C:24]=2[NH:26][C:27](=[O:28])[CH2:29]1.[OH2:31]

参加物

4

反応物 2

HCID 962WaterHCID 60795Aripiprazole2 回

生成物 1

HCID 114086887-{4-[4-(2,3-dichlorophenyl)piperazin-1-yl]butoxy}-1,2,3,4-tetrahydroquinolin-2-one hydrate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The resulting crude aripiprazole (aripiprazole anhydrous crystal) was added to water-containing ethanol (ethanol: 80%, water: 20%), and heated to a solvent reflux temperature to completely dissolve the crude aripiprazole. The solution was cooled to precipitate an aripiprazole hydrate crystal, and the aripiprazole hydrate crystal was precipitated and milled by a wet pulverization device. After the solvent was removed by filtration, drying (air-drying overnight at room temperature) was performed to obtain an aripiprazole hydrate fine crystal (a crystal of aripiprazole hydrate A). The particle size was adjusted by wet pulverization operation conditions (suspension temperature, rotation speed, shape of wings for pulverization, etc.) to prepare a crystal of aripiprazole hydrate A having a desired particle size.

後処理

  1. temperatureheated to a solvent
  2. temperaturereflux temperature
  3. temperatureThe solution was cooled
  4. customto precipitate an aripiprazole hydrate crystal
  5. customthe aripiprazole hydrate crystal was precipitated
  6. custommilled by a wet pulverization device
  7. customAfter the solvent was removed by filtration
  8. customdrying
  9. custom(air-drying overnight at room temperature)

出典と根拠

ORDレコード
ord-7b1e8b7040d94221b4920a6ca5eb3898
出典データセット
uspto-grants-2015_06
特許番号
US09051268B2

反応ノート

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