Potassium Iodide → 1-[4-(4-Benzo[d]isothiazol-3-yl-piperazin-1-yl)-butyl]-4,4-dimethyl-piperidine-2,6-dione

HRID 648199

反応式

HRID 648199 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[C:11](=[O:12])[CH2:10][C:9]([CH3:14])([CH3:13])[CH2:8][C:7]1=[O:15].[N:16]1([C:22]2[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[S:24][N:23]=2)[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>C(#N)C>[S:24]1[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[C:22]([N:16]2[CH2:17][CH2:18][N:19]([CH2:2][CH2:3][CH2:4][CH2:5][N:6]3[C:11](=[O:12])[CH2:10][C:9]([CH3:14])([CH3:13])[CH2:8][C:7]3=[O:15])[CH2:20][CH2:21]2)=[N:23]1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 27721443-(1-Piperazinyl)-1,2-benzisothiazoleHCID 136603351-(4-Bromobutyl)-4,4-dimethylpiperidine-2,6-dione

生成物 1

HCID 132324931-[4-(4-Benzo[d]isothiazol-3-yl-piperazin-1-yl)-butyl]-4,4-dimethyl-piperidine-2,6-dione収率 64%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of N-(4-bromobutyl)-3,3-dimethylglutarimide (4 g., 0.0145 mole) obtained according to the procedure of Example 9, 3-(1-piperazinyl)-1,2-benzisothiazole (3.18 g., 0.0145 mole), anhydrous potassium carbonate (20.04 g., 0.145 mole) and potassium iodide (0.25 g., 0.0015 mole) in 150 ml. of acetonitrile is stirred and refluxed for a period of 12 hr. The reaction mixture is filtered, concentrated in vacuo and residual material triturated with ether. Crystallization of the solid thus obtained from ether affords a 64% yield of analytically pure 1-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]butyl]-4,4-dimethyl-2,6-piperidinedione, m.p. 146°-147° C.

後処理

  1. customobtained
  2. temperaturerefluxed for a period of 12 hr
  3. filtrationThe reaction mixture is filtered
  4. concentrationconcentrated in vacuo and residual material
  5. customtriturated with ether
  6. customCrystallization of the solid
  7. customthus obtained from ether

出典と根拠

ORDレコード
ord-5dc039cc55534781a6a3962d342d7d59
出典データセット
uspto-grants-1983_10
特許番号
US04411901

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