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

HRID 704883Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 704883
Br[CH2:2][CH2:3][CH2:4][N:5]1[C:10](=[O:11])[NH:9][C:8]2[CH:12]=[CH:13][C:14]([O:16][CH3:17])=[CH:15][C:7]=2[S:6]1(=[O:19])=[O:18].[N:20]1[CH:25]=[CH:24][CH:23]=[N:22][C:21]=1[N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.C(N(CC)CC)C.O>CN(C=O)C>[N:20]1[CH:25]=[CH:24][CH:23]=[N:22][C:21]=1[N:26]1[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][N:5]2[C:10](=[O:11])[NH:9][C:8]3[CH:12]=[CH:13][C:14]([O:16][CH3:17])=[CH:15][C:7]=3[S:6]2(=[O:19])=[O:18])[CH2:28][CH2:27]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 887471-(2-Pyrimidinyl)piperazineHCID 190234312-(3-bromopropyl)-7-methoxy-1,2,4-benzothiadiazin-3(4H)one 1,1-dioxide

Produkt 1

HCID 190234012-(3-(4-(2-pyrimidinyl)-1-piperazinyl)propyl)-7-methoxy-1,2,4-benzothiadiazin-3(4H)one 1,1dioxide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

0.01 mol of 2-(3-bromopropyl)-7-methoxy-1,2,4benzothiadiazin-3(4H)one 1,1-dioxide, 0.012 mol of 1-(2pyrimidinyl)piperazine and 0.01 mol of triethylamine are dissolved in 30 ml of DMF and the solution is heated at 60° C., with stirring, for 1.5 hours. Then 15 ml of water are added and the reaction mixture is cooled to 0° C. The substance which crystallises out during this is filtered off with suction, stirred with isopropanol, again filtered off with suction and dried in vacuo.

Aufarbeitung

  1. temperaturethe reaction mixture is cooled to 0° C
  2. customThe substance which crystallises out during
  3. filtrationthis is filtered off with suction
  4. stirringstirred with isopropanol
  5. filtrationagain filtered off with suction
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-1e8f8854e5ca461aa6b15ee81b8ca2df
Quelldatensatz
uspto-grants-1991_01
Patentnummer
US04988809

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