反应详情

温度

75 °C

In a 50 mL heavy walled glass pressure flask 4-methoxy-6-(4-methoxybenzyl)-N,N,2-trimethyl-3,5-dioxo-2,3,5,6,7,8-hexahydro-2,6-naphthyridine-1-carboxamide (3.9 g) and 15 ml of (commercial) 33% HBr in HOAc were mixed. The flask was sealed, heated to 75° C. and allowed to stir overnight. The solvent was removed in vacuo. The remaining oil was dissolved in CH3CN and purified by reverse phase on a Biotage KPCM 250 compression module containing a 10 cm×60 cm Kiloprep cartridge. The product elutes at 13% CH3CN in water containing 0.1% TFA.

1. additionwere mixed
2. customThe flask was sealed
3. customThe solvent was removed in vacuo
4. dissolutionThe remaining oil was dissolved in CH3CN
5. custompurified by reverse phase on a Biotage KPCM 250 compression module
6. additioncontaining a 10 cm×60 cm Kiloprep cartridge