반응 #46271

반응 방정식

methyl 2-(4-chlorobutyl)-6-(3-chloro-4-fluorobenzyl)-4-hydroxy-3,5-dioxo-2,3,5,6,7,8-hexahydro-2,6-naphthyridine-1-carboxylate

methylamine

→

title compound

Methyl 6-(3-chloro-4-fluorobenzyl)-4-hydroxy-2-[4-(methylamino)butyl]-3,5-dioxo-2,3,5,6,7,8-hexahydro-2,6-naphthyridine-1-carboxylate

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated under vacuum
2. 2
   기타The residue was partitioned between dichloromethane and saturated aqueous sodium bicarbonate
3. 3
   추출The organic extract
4. 4
   세척was washed with brine
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated under vacuum

실험 절차

A mixture of methyl 2-(4-chlorobutyl)-6-(3-chloro-4-fluorobenzyl)-4-hydroxy-3,5-dioxo-2,3,5,6,7,8-hexahydro-2,6-naphthyridine-1-carboxylate (0.10 g, 0.21 mmol), methylamine in tetrahydrofuran (1 mL, 2M), and tetra-n-butylammonium iodide in tetrahydrofuran (5 mL) was heated at 60° C. for 3 days. The reaction mixture was concentrated under vacuum. The residue was partitioned between dichloromethane and saturated aqueous sodium bicarbonate. The organic extract was washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated under vacuum to provide the title compound. This was used in the following step without further purification.

출처