反应详情

温度

60 °C

Ethyl 6-chloro-4-hydroxy-1,1-dimethyl-2-oxo-naphthalene-3-carboxylate (1.10 g, 3732 μmol, see Example 2) was dissolved in 2M methanamine in THF (9331 μL, 18661 μmol). The resulting mixture was stirred at 60° C. for 16 hours and then diluted with 100 mL of EtOAc. The resulting mixture was added to a separatory funnel, partitioned with NaHCO3 (saturated, aqueous), washed 2 times with 20 mL of NaHCO3 (saturated, aqueous), separated, dried over Na2SO4 and concentrated in vacuo to give the title compound (131 mg) as a white solid after purification via preparatory LC. MS m/e=280 (M+H)+. Calculated for C14H14ClNO3 279.07.

1. additionThe resulting mixture was added to a separatory funnel
2. custompartitioned with NaHCO3 (saturated, aqueous)
3. washwashed 2 times with 20 mL of NaHCO3 (saturated, aqueous)
4. customseparated
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo