Acetone → 4-amino-5-chloro-2-[2-(methylsulfinyl)ethoxy]-N-[2-(diethylamino)ethyl]benzamide hydrochloride monohydrate

HRID 620289

Reaktionsgleichung

[NH2:1][C:2]1[C:17]([Cl:18])=[CH:16][C:5]([C:6]([NH:8][CH2:9][CH2:10][N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])=[O:7])=[C:4]([O:19][CH2:20][CH2:21][S:22]([CH3:24])=[O:23])[CH:3]=1.CC(C)=O.Cl>CC(O)C>[OH2:7].[ClH:18].[NH2:1][C:2]1[C:17]([Cl:18])=[CH:16][C:5]([C:6]([NH:8][CH2:9][CH2:10][N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])=[O:7])=[C:4]([O:19][CH2:20][CH2:21][S:22]([CH3:24])=[O:23])[CH:3]=1

Komponenten

Reaktionsbedingungen

Temperatur: 25 °C

Versuchsvorschrift

A mixture of 4-amino-5-chloro-2[2-(methylsulfinyl)ethoxy]-N-[2-(diethylamino)ethyl]benzamide (84.50 g, 22.5 mmoles), acetone (592 ml) and 2-propanol (169 ml) was stirred and warmed until complete solution (ca. 25° C.) and then 56.2 ml of 4N HCl (1 equivalent) was all at once. The temperature rose to 32° C. After one hour at ambient temperature the mixture was stored at 0° C. for 18 hours. The hydrochloride salt was collected by filtration, rinses with acetone and dried in vacuo over P2O5 for six hours. Yield: 89.6 g (96.6%); mp 117°-124° C.

Aufarbeitung

customrose to 32° C
filtrationThe hydrochloride salt was collected by filtration, rinses with acetone
dry with materialdried in vacuo over P2O5 for six hours

Quellen und Nachweise

ORD-Eintrag: ord-0cdd82d3d03e4f99b4b7d037fb45ca38
Quelldatensatz: uspto-grants-1989_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04820715

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