反应详情

N-(3,4-Dichlorophenyl)piperazine-1-carboxamide hydrochloride (467 mg) and 4-(tert-butoxycarbonyl)morpholine-2-carboxylic acid (347 mg) were dissolved in dry THF (10 mL) followed by addition of N,N-diisopropylethylamine (0.52 ml) and HATU (628 mg) and the reaction was stirred for 4 h. The solvent was evaporated under reduced pressure then redissolved in ethyl acetate (50 ml) followed by washing with sat. aqueous NaHCO3 (20 ml), 10% w/v citric acid (aq.) (15 ml) and brine (15 ml). The organic layer was dried (MgSO4), filtered and evaporated. Purification by chromatography (1:1 EtOAc:hexanes 1:1 to EtOAc neat) afforded the title compound (900 mg) as an impure foam contaminated with N,N,N′,N′-tetramethylurea. The product was used without further purification.

1. customThe solvent was evaporated under reduced pressure
2. dissolutionthen redissolved in ethyl acetate (50 ml)
3. washby washing with sat. aqueous NaHCO3 (20 ml), 10%
4. dry with materialThe organic layer was dried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customPurification by chromatography (1:1 EtOAc:hexanes 1:1 to EtOAc neat)