乙基 2-[(2-甲氧基-2-氧乙基)氨基]-2-氧代乙酸乙酯

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of ethyl 2-(2-methoxy-2-oxoethylamino)-2-oxoacetate (1.00 g, 5.29 mmol) and phosphorus pentasulfide (1.29 g, 5.82 mmol) in chloroform (20 ml) was stirred at 60° C. for 7 h. To the cooled reaction mixture DCM (100 ml) was added and the mixture was washed with water (50 ml) and brine (50 ml). Organic phase was dried over Na2SO4 and evaporated. Evaporation residual was dissolved in dry MeCN (10 ml) and phosphorus pentoxide (0.75 g, 5.29 mml) was added and the mixture was heated to reflux for 4.5 h. To the cooled reaction mixture water (35 ml) was added and the mixture was extracted with EtOAc (3×50 ml). Combined organic fractions were dried over Na2SO4 and evaporated to give crude product, which was purified twice by CombiFlash (1st column: silica, eluent: 0-100% EtOAc in heptane; 2nd column: C-18, eluent: 0-100% MeCN in water) to yield 73 mg (7%) of the title compound. 1H-NMR (400 MHz; CDCl3): δ 1.42 (t, 3H), 4.01 (s, 3H), 4.43 (q, 2H), 7.30 (s, 1H). was added the mixture was washed with water (50 ml) and brine (50 ml) Organic phase was dried over Na2SO4 evaporated Evaporation residual was dissolved in dry MeCN (10 ml) phosphorus pentoxide (0.75 g, 5.29 mml) was added the mixture was heated to reflux for 4.5 h To the cooled reaction mixture water (35 ml) was added the mixture was extracted with EtOAc (3×50 ml) Combined organic fractions were dried over Na2SO4 evaporated to give crude product, which was purified twice by CombiFlash (1st column: silica, eluent: 0-100% EtOAc in heptane; 2nd column: C-18, eluent: 0-100% MeCN in water)

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of ethyl 2-(2-methoxy-2-oxoethylamino)-2-oxoacetate (1.00 g, 5.29 mmol) and phosphorus pentasulfide (1.29 g, 5.82 mmol) in chloroform (20 ml) was stirred at 60° C. for 7 h. To the cooled reaction mixture DCM (100 ml) was added and the mixture was washed with water (50 ml) and brine (50 ml). Organic phase was dried over Na2SO4 and evaporated. Evaporation residual was dissolved in dry MeCN (10 ml) and phosphorus pentoxide (0.75 g, 5.29 mml) was added and the mixture was heated to reflux for 4.5 h. To the cooled reaction mixture water (35 ml) was added and the mixture was extracted with EtOAc (3×50 ml). Combined organic fractions were dried over Na2SO4 and evaporated to give crude product, which was purified twice by CombiFlash (1st column: silica, eluent: 0-100% EtOAc in heptane; 2nd column: C-18, eluent: 0-100% MeCN in water) to yield 73 mg (7%) of the title compound. 1H-NMR (400 MHz; CDCl3): δ 1.42 (t, 3H), 4.01 (s, 3H), 4.43 (q, 2H), 7.30 (s, 1H). was added the mixture was washed with water (50 ml) and brine (50 ml) Organic phase was dried over Na2SO4 evaporated Evaporation residual was dissolved in dry MeCN (10 ml) phosphorus pentoxide (0.75 g, 5.29 mml) was added the mixture was heated to reflux for 4.5 h To the cooled reaction mixture water (35 ml) was added the mixture was extracted with EtOAc (3×50 ml) Combined organic fractions were dried over Na2SO4 evaporated to give crude product, which was purified twice by CombiFlash (1st column: silica, eluent: 0-100% EtOAc in heptane; 2nd column: C-18, eluent: 0-100% MeCN in water)