Hydrochloric Acid → Zolpidem hydrochloride

HRID 1066183

반응식

HRID 1066183 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:16]=[C:15]3[N:10]([CH:11]=[C:12]([CH3:17])[CH:13]=[CH:14]3)[C:9]=2[CH2:18][C:19]([N:21]([CH3:23])[CH3:22])=[O:20])=[CH:6][CH:7]=1.[ClH:24]>C(O)CCC>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:16]=[C:15]3[N:10]([CH:11]=[C:12]([CH3:17])[CH:13]=[CH:14]3)[C:9]=2[CH2:18][C:19]([N:21]([CH3:22])[CH3:23])=[O:20])=[CH:4][CH:3]=1.[ClH:24]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 5732Zolpidem

생성물 1

HCID 18004031Zolpidem hydrochloride

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

One gram of zolpidem is suspended in 35 ml of 1-butanol, 0.32 g of concentrated hydrochloric acid is added and the mixture stirred 15 minutes at room temperature. The clear solution is heated to reflux and 25 ml of a water/1-butanol mixture is distilled off. The resulting mixture is allowed to cool to room temperature and stirred at room temperature for 16 hours. The formed solid is filtered off, washed with 2 ml of 1-butanol and dried in a vacuum oven at 40° C. to produce zolpidem hydrochloride anhydrate. A representative DSC curve is shown in FIG. 11.

후처리

  1. temperatureThe clear solution is heated
  2. temperatureto reflux
  3. distillation25 ml of a water/1-butanol mixture is distilled off
  4. temperatureto cool to room temperature
  5. stirringstirred at room temperature for 16 hours
  6. filtrationThe formed solid is filtered off
  7. washwashed with 2 ml of 1-butanol
  8. customdried in a vacuum oven at 40° C.

출처 및 근거

ORD 기록
ord-867bfc6d27514615bf014daebcce4be2
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06242460B1

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