benzyl 2-[2-(methylcarbamoyl)morpholin-4-yl]acetate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: benzyl 2-(2-(methylcarbamoyl)morpholino)acetate was dissolved in ethanol (40 mL), Pd/C 10% (100 mg) was added to the solution, and the mixture was stirred overnight under hydrogen (balloon) then filtered through celite and concentrated to give 2-(2-(methylcarbamoyl)morpholino)acetic acid. MS (APCI) 203 (M+1) then filtered through celite and concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: benzyl 2-(2-(methylcarbamoyl)morpholino)acetate was dissolved in ethanol (40 mL), Pd/C 10% (100 mg) was added to the solution, and the mixture was stirred overnight under hydrogen (balloon) then filtered through celite and concentrated to give 2-(2-(methylcarbamoyl)morpholino)acetic acid. MS (APCI) 203 (M+1) then filtered through celite and concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: tert-butyl 2-(methylcarbamoyl)morpholine-4-carboxylate prepared above (0.5 g, 0.20 mmol) was dissolved in DCM (10 mL) and TFA (2 mL). The reaction mixture was stirred at room temperature for 4 h and then concentrated; excess 1N HCl solution in ether was added to the residue and concentrated under high vacuum. The residue was dissolved in acetonitrile (20 mL) and K2CO3 (0.56 g, 40.8 mmol) was added followed by bromo-acetic acid benzyl ester (0.7 g, 3.07 mmol). The reaction mixture was heated at 60° C. overnight. The solution was cooled to room temperature and diluted with Ethyl acetate (50 mL) and water (50 mL), organic layer was separated, dried (MgSO4) and concentrated to give an oil which was purified by column chromatography using ethyl acetate-hexanes (1:1) to give benzyl 2-(2-(methylcarbamoyl)morpholino)acetate. MS (APCI) 293 (M+). concentrated excess 1N HCl solution in ether was added to the residue concentrated under high vacuum The residue was dissolved in acetonitrile (20 mL) The reaction mixture was heated at 60° C. overnight The solution was cooled to room temperature was separated dried (MgSO4) concentrated to give an oil which was purified by column chromatography

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: benzyl 2-(2-(methylcarbamoyl)morpholino)acetate was dissolved in ethanol (40 mL), Pd/C 10% (100 mg) was added to the solution, and the mixture was stirred overnight under hydrogen (balloon) then filtered through celite and concentrated to give 2-(2-(methylcarbamoyl)morpholino)acetic acid. MS (APCI) 203 (M+1) then filtered through celite and concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: tert-butyl 2-(methylcarbamoyl)morpholine-4-carboxylate prepared above (0.5 g, 0.20 mmol) was dissolved in DCM (10 mL) and TFA (2 mL). The reaction mixture was stirred at room temperature for 4 h and then concentrated; excess 1N HCl solution in ether was added to the residue and concentrated under high vacuum. The residue was dissolved in acetonitrile (20 mL) and K2CO3 (0.56 g, 40.8 mmol) was added followed by bromo-acetic acid benzyl ester (0.7 g, 3.07 mmol). The reaction mixture was heated at 60° C. overnight. The solution was cooled to room temperature and diluted with Ethyl acetate (50 mL) and water (50 mL), organic layer was separated, dried (MgSO4) and concentrated to give an oil which was purified by column chromatography using ethyl acetate-hexanes (1:1) to give benzyl 2-(2-(methylcarbamoyl)morpholino)acetate. MS (APCI) 293 (M+). concentrated excess 1N HCl solution in ether was added to the residue concentrated under high vacuum The residue was dissolved in acetonitrile (20 mL) The reaction mixture was heated at 60° C. overnight The solution was cooled to room temperature was separated dried (MgSO4) concentrated to give an oil which was purified by column chromatography