Potassium Carbonate → Ziprasidone

HRID 13567

반응식

HRID 13567 반응식
[N:1]1([C:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[S:9][N:8]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[Cl:16][C:17]1[CH:25]=[C:24]2[C:20]([CH2:21][C:22](=[O:26])[NH:23]2)=[CH:19][C:18]=1[CH2:27][CH2:28]Cl.C(=O)([O-])[O-].[K+].[K+].S1(CCCC1)(=O)=O>[I-].[K+].O>[S:9]1[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:7]([N:1]2[CH2:6][CH2:5][N:4]([CH2:28][CH2:27][C:18]3[CH:19]=[C:20]4[C:24](=[CH:25][C:17]=3[Cl:16])[NH:23][C:22](=[O:26])[CH2:21]4)[CH2:3][CH2:2]2)=[N:8]1

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 31347SulfolaneHCID 27721443-(1-Piperazinyl)-1,2-benzisothiazoleHCID 106094745-(2-Chloroethyl)-6-chlorooxindole

생성물 1

HCID 60854Ziprasidone수율 74.8%

시약·촉매·용매 2

HCID 4875Potassium Iodide촉매HCID 962Water용매

실험 절차

In glass-lined reactor placed 21.1 Kg (96.34 mole) of 3-piperazinylbenzo[d]isothiazole; 31 kg (134.7 moles) of 6-chloro-5-(2-chloroethyl)indolin-2-one; 1.1 kg of potassium iodide; 20.0 kg (111.92 mole) of potassium carbonate and 63.2 lit of sulfolane. The contents of the flask were initially heated to 75° C. to 80° C. for 2 hrs. Then temperature was raised to 95° C. to 100° C. and stirred till completion of the reaction. After completion of the reaction 210 lit of DM water was added to the reaction mixture and stirred. The product was filtered off and washed with water and dried to obtain 29.75 kg of 5-(2-(4-(1,2-benzisothiazol-3-yl)-1-piperazinyl)ethyl)-6-chloro-1,3-dihydro-2H-indol-2-one (Ziprasidone).

후처리

  1. customIn glass-lined reactor placed
  2. temperatureThe contents of the flask were initially heated to 75° C. to 80° C. for 2 hrs
  3. temperatureThen temperature was raised to 95° C. to 100° C.
  4. additionwas added to the reaction mixture
  5. stirringstirred
  6. filtrationThe product was filtered off
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-1f25ff321e514b58b4c5fca27a5d1686
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728136B2

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