Diethyl Ether → Quetiapine Besylate

HRID 421568

反応式

HRID 421568 の反応式
[CH:1]1[CH:2]=[CH:3][C:4]2[S:15][C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[N:8]=[C:7]([N:16]3[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][O:24][CH2:25][CH2:26][OH:27])[CH2:18][CH2:17]3)[C:5]=2[CH:6]=1.[C:28]1([S:34]([OH:37])(=[O:36])=[O:35])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.C(OCC)C>CC(C)=O>[CH:1]1[CH:2]=[CH:3][C:4]2[S:15][C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[N:8]=[C:7]([N:16]3[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][O:24][CH2:25][CH2:26][OH:27])[CH2:18][CH2:17]3)[C:5]=2[CH:6]=1.[S:34]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)([O-:37])(=[O:36])=[O:35]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 5002QuetiapineHCID 7371Benzenesulfonic Acid

生成物 1

HCID 131729401Quetiapine Besylate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
42.5 °C

実験手順

Quetiapine free base (5.0 g) was dissolved in acetone (50 ml) at room temperature. This was followed by the addition of benzene sulfonic acid (2.0 g) at 30 to 35° C. The resulting mass was heated at 40-45° C. and maintained for 30 minutes. The resulting mass was cooled at 25-30° C. This was followed by the addition of diethyl ether (50 ml) and stirred for 3 hours. The precipitated product was collected by filtration under nitrogen and washed with diethyl ether (25 ml) and dried under vacuum to give the title compound as off white powder (5.94 g).

後処理

  1. temperaturemaintained for 30 minutes
  2. temperatureThe resulting mass was cooled at 25-30° C
  3. filtrationThe precipitated product was collected by filtration under nitrogen
  4. washwashed with diethyl ether (25 ml)
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-c659196a311943ae9e9e81e03e4b6e1a
出典データセット
uspto-grants-2012_01
特許番号
US08101597B2

関連ノート

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