Methyl iodide → 2-(3-(4-(2-pyrimidinyl)-1-piperazinyl)propyl)-4-methyl-7-methoxy-1,2,4-benzothiadiazin-3(4H)one 1,1-dioxide

HRID 704884Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 704884
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][N:16]2[C:21](=[O:22])[NH:20][C:19]3[CH:23]=[CH:24][C:25]([O:27][CH3:28])=[CH:26][C:18]=3[S:17]2(=[O:30])=[O:29])[CH2:9][CH2:8]1.[H-].[Na+].[CH3:33]I>CN(C=O)C>[N:3]1[CH:4]=[CH:5][CH:6]=[N:1][C:2]=1[N:7]1[CH2:8][CH2:9][N:10]([CH2:13][CH2:14][CH2:15][N:16]2[C:21](=[O:22])[N:20]([CH3:33])[C:19]3[CH:23]=[CH:24][C:25]([O:27][CH3:28])=[CH:26][C:18]=3[S:17]2(=[O:29])=[O:30])[CH2:11][CH2:12]1

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 190234012-(3-(4-(2-pyrimidinyl)-1-piperazinyl)propyl)-7-methoxy-1,2,4-benzothiadiazin-3(4H)one 1,1dioxide

Produkt 1

HCID 190234672-(3-(4-(2-pyrimidinyl)-1-piperazinyl)propyl)-4-methyl-7-methoxy-1,2,4-benzothiadiazin-3(4H)one 1,1-dioxide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

0.028 mol of 2-(3-(4-(2-pyrimidinyl)-1-piperazinyl)propyl)-7-methoxy-1,2,4-benzothiadiazin-3(4H)one 1,1dioxide is dissolved in 150 ml of absolute DMF, and 0.028 mol of sodium hydride is added to the solution and the mixture is stirred at room temperature for 0.25 hour. Then 0.028 mol of methyl iodide is added and the mixture is stirred at 25° C. for a further 2 hours. The product is precipitated as crystals by dropwise addition of a total of 18 ml of water. It is purified by crystallisation from isopropanol.

Aufarbeitung

  1. stirringthe mixture is stirred at 25° C. for a further 2 hours
  2. customThe product is precipitated as crystals by dropwise addition of a total of 18 ml of water
  3. customIt is purified by crystallisation from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-15a1f05c59064591afee1a9a511ffb1e
Quelldatensatz
uspto-grants-1991_01
Patentnummer
US04988809

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