Hydrochloric Acid → Ziprasidone Hydrochloride

HRID 547881

반응식

HRID 547881 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([N:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][C:18]3[CH:19]=[C:20]4[C:24](=[CH:25][C:26]=3[Cl:27])[NH:23][C:22](=[O:28])[CH2:21]4)[CH2:12][CH2:11]2)=[N:2]1.[Cl:29]CCl.Cl>C(O)(C)C>[CH:8]1[CH:7]=[CH:6][C:5]2[S:1][N:2]=[C:3]([N:10]3[CH2:11][CH2:12][N:13]([CH2:16][CH2:17][C:18]4[CH:19]=[C:20]5[CH2:21][C:22](=[O:28])[NH:23][C:24]5=[CH:25][C:26]=4[Cl:27])[CH2:14][CH2:15]3)[C:4]=2[CH:9]=1.[ClH:29]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 60854Ziprasidone

생성물 1

HCID 219099Ziprasidone Hydrochloride

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
22.5 °C

실험 절차

To a flask equipped with magnetic stirrer, thermometer and nitrogen inlet was added 5-(2-(4-(1,2-benzisothiazol-3-yl)-1-piperazinyl)ethyl)-6-chloro-1,3-dihydro-2H-indol-2-one free base (5.0 g) and dichloromethane (100 mL) and the suspension was stirred at 20-25° C. under nitrogen. A 20.5% anhydrous solution of hydrogen chloride in isopropanol (6.45 g) was added and the mixture was stirred for about 2 h. The product was collected by filtration on a Buchner funnel. The filter cake is rinsed with 3×10 mL of dichloromethane at 20-25° C. and transferred to a drying oven and dried in vacuo at 65-70° C. for about 18 h. The crude material was re-slurried at 20-25° C. for 10 minutes with heptanes and the suspension was filtered in vacuo. The filter cake is rinsed with heptanes at 20-25° C. and transferred to a drying oven and dried in vacuo at 65-70° C. for about 12 h. to afford amorphous ziprasidone hydrochloride having the same PXRD diffractogram, IR and DSC as shown in FIGS. 1 to 3.

후처리

  1. customTo a flask equipped with magnetic stirrer
  2. stirringthe mixture was stirred for about 2 h
  3. filtrationThe product was collected by filtration on a Buchner funnel
  4. washThe filter cake is rinsed with 3×10 mL of dichloromethane at 20-25° C.
  5. customtransferred to a drying oven
  6. customdried in vacuo at 65-70° C. for about 18 h
  7. filtrationthe suspension was filtered in vacuo
  8. washThe filter cake is rinsed with heptanes at 20-25° C.
  9. customtransferred to a drying oven
  10. customdried in vacuo at 65-70° C. for about 12 h.

출처 및 근거

ORD 기록
ord-a21f5907ef164a52a850f141c98ce32c
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07939662B2

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