Reaktion #11519

Reaktionsgleichung

ammonia

trichloroacetylisocyanate

2-Amino-4-methyl-5-(1,4-benzodioxan-6-yl)-3-thiophencarboxamide

→

2-[(Aminocarbonyl)amino]-4-methyl-5-(1,4-benzodioxan-6-yl)-3-thiophenecarboxamide

Lösungsmittel

methanol

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGStirring
2. 2
   workup.STIRRINGstirring
3. 3
   workup.WAITwas continued for a further 3 h
4. 4
   SonstigeThe solvent was evaporated
5. 5
   workup.ADDITIONthe residue treated with ethyl acetate
6. 6
   Filtrationthe product filtered off

Vorschrift

2-Amino-4-methyl-5-(1,4-benzodioxan-6-yl)-3-thiophencarboxamide (0.44 g) was dissolved in tetrahydrofuran (10 ml), cooled to 0° C. and trichloroacetylisocyanate (0.11 ml) added dropwise with stirring. Stirring was continued for a further 30 minutes at room temperature and then a solution of ammonia in methanol (8 ml of a 10% solution) was added and stirring was continued for a further 3 h. The solvent was evaporated and the residue treated with ethyl acetate and the product filtered off.

Quelle