Reaktion #512418

Reaktionsgleichung

ethanol

N-((S)-3-bromo-2-hydroxypropyl)-5-chlorothiophene-2-carboxamide

N-((S)-3-Bromo-2-hydroxypropyl)-5-chlorothiophene-2-carboxamide

4-(4-aminophenyl)-3-morpholinone

collidine

→

N-{(R)-2-Hydroxy-3-[4-(3-oxomorpholin-4-yl)phenylamino]propyl}-5-chloro-thiophene-2-carboxamide

Lösungsmittel

1-butanol

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling to 30° C.
2. 2
   Sonstigethe precipitated reaction product
3. 3
   Filtrationis filtered off with suction
4. 4
   Waschenwashed with toluene and water
5. 5
   Sonstigedried

Vorschrift

55 g of N-((S)-3-bromo-2-hydroxypropyl)-5-chlorothiophene-2-carboxamide (IX) and 29.4 g of 4-(4-aminophenyl)-3-morpholinone (III) (a preparation method is described, for example, in WO-A 01/47919 on pages 55 to 57) are suspended at from 20 to 25° C. in 500 ml of toluene and admixed with 18.5 g of collidine and 10 ml of ethanol. The reaction mixture is heated to from 103 to 105° C. for 6 hours and then admixed while hot with 50 ml of 1-butanol. After cooling to 30° C., the precipitated reaction product is filtered off with suction, washed with toluene and water and dried.

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