Potassium Carbonate → Ziprasidone

HRID 13567

反応式

HRID 13567 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 60854Ziprasidone収率 74.8%

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide触媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1f25ff321e514b58b4c5fca27a5d1686
出典データセット
uspto-grants-2010_06
特許番号
US07728136B2

関連ノート

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