Hydrogen Bromide → Quetiapine Hydrobromide

HRID 421566

반응식

HRID 421566 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.[BrH:28]>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.[BrH:28]

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 5002Quetiapine

생성물 1

HCID 24748093Quetiapine Hydrobromide

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
22.5 °C

실험 절차

Quetiapine free base (5.0 g) was dissolved in acetone (50 ml) at room temperature. This was followed by addition of 48% aqueous hydrobromic acid (2 ml) at 30 to 35° C. The resulting solution was stirred for 1 hour at 20 to 25° C. Next, acetone was distilled under vacuum at 40 to 45° C. followed by addition of acetone (50 ml) and distilled under vacuum at 40 to 45° C. till complete removal. Next, acetone (50 ml) and diisopropyl ether (50 ml) were added at 40 to 45° C. The resulted mass was refluxed for 30 minutes and cooled at 20 to 25° C. and further stirred for 2.5 hours. The precipitated product was collected by filtration, washed with diisopropyl ether (25 ml) and dried to give the title compound as white powder (3.8 g).

후처리

  1. distillationNext, acetone was distilled under vacuum at 40 to 45° C.
  2. additionfollowed by addition of acetone (50 ml)
  3. distillationdistilled under vacuum at 40 to 45° C. till complete removal
  4. additionNext, acetone (50 ml) and diisopropyl ether (50 ml) were added at 40 to 45° C
  5. temperatureThe resulted mass was refluxed for 30 minutes
  6. temperaturecooled at 20 to 25° C.
  7. stirringfurther stirred for 2.5 hours
  8. filtrationThe precipitated product was collected by filtration
  9. washwashed with diisopropyl ether (25 ml)
  10. customdried

출처 및 근거

ORD 기록
ord-53e519a6384e42af952748f71bb5e7de
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101597B2

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