Hydrochloric Acid → 5-(4-Methyl-4-oxidopiperazino)-imidazo[2,1-b][1,3,5]benzothiadiazepine hydrochloride

HRID 1074409

Reaktionsgleichung

Reaktionsgleichung von HRID 1074409
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[N:9]3[CH:21]=[CH:20][N:19]=[C:10]3[S:11][C:12]3[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=3[N:14]=2)[CH2:4][CH2:3]1.[Cl:22]C1C=CC=C(C(OO)=[O:30])C=1.Cl>C(Cl)Cl.CCOCC>[ClH:22].[CH3:1][N+:2]1([O-:30])[CH2:7][CH2:6][N:5]([C:8]2[N:9]3[CH:21]=[CH:20][N:19]=[C:10]3[S:11][C:12]3[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=3[N:14]=2)[CH2:4][CH2:3]1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 54742PentiapineHCID 70297m-Chloroperbenzoic acid

Produkt 1

HCID 155864195-(4-Methyl-4-oxidopiperazino)-imidazo[2,1-b][1,3,5]benzothiadiazepine hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To the solution of 88 mg of 5-(4-methylpiperazino)-imidazo[2,1-b][1,3,5]benzothiadiazepine in 1 ml of methylene chloride, 74 mg of m-chloroperbenzoic acid are added at 0° C. The mixture is stirred at 0° C. overnight; this is diluted with 1 ml of ether, one equivalent of ethereal hydrochloric acid solution is added and the resulting precipitate is collected. Recrystallization from methanol-ethyl acetate yields 5-(4-methyl-4-oxidopiperazino)-imidazo[2,1-b][1,3,5]benzothiadiazepine hydrochloride, melting at 155° with decomposition.

Aufarbeitung

  1. additionis added
  2. customthe resulting precipitate is collected
  3. customRecrystallization from methanol-ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-bd76b2b5f6484aedb9e1051a75695721
Quelldatensatz
uspto-grants-1983_07
Patentnummer
US04391808

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