Diethyl Ether → Quetiapine Besylate

HRID 421568

반응식

HRID 421568 반응식
[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]

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 5002QuetiapineHCID 7371Benzenesulfonic Acid

생성물 1

HCID 131729401Quetiapine Besylate

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
42.5 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c659196a311943ae9e9e81e03e4b6e1a
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101597B2

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