反应详情

温度

80 °C

Ethyl 4-hydroxy-1,1-dimethyl-2-oxo-naphthalene-3-carboxylate (425 mg, 1633 μmol) was dissolved in 1,4-dioxane (1633 μL) and N-ethyl-N-isopropylpropan-2-amine (853 μL, 4898 μmol). tert-Butyl 2-aminoacetate hydrochloride (411 mg, 2449 μmol) was added, and the mixture was heated at 80° C. for 4 hours. The reaction mixture was then cooled, diluted with 100 mL of EtOAc, added to a separatory funnel, partitioned with NaHCO3 (saturated, aqueous), washed 2 times with 50 mL of NaHCO3 (saturated, aqueous), separated, dried over Na2SO4, and concentrated in vacuo to give the title compound (279 mg) as a white solid after purification via preparatory LC. MS (m/z)=290 (M+H-tBu)+.

1. temperatureThe reaction mixture was then cooled
2. additionadded to a separatory funnel
3. custompartitioned with NaHCO3 (saturated, aqueous)
4. washwashed 2 times with 50 mL of NaHCO3 (saturated, aqueous)
5. customseparated
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo