N,N-二甲基-2-氧代丙酰胺

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: A mixture of 1-(o-hydroxyphenyl)pyrrole (500 mg), N,N-dimethyl-pyruvamide (580 mg), described by W. F. Gresham in U.S. Pat. No. 2,429,877, issued Oct. 28, 1947, 1.7 g of phosphorus pentoxide, 0.5 g of diatomaceous earth (Celite) in 75 ml of benzene is stirred at room temperature for 15 min. and then at 70° C for 11/2 hr. The reaction mixture is filtered. The filtrate is washed with water, dried (MgSO4) and concentrated to give the title compound, identical to the product of Example 15. at 70° C 2 hr The reaction mixture is filtered The filtrate is washed with water dried (MgSO4) concentrated

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

实验步骤: A mixture of 1-(o-hydroxyphenyl)pyrrole (500 mg), N,N-dimethyl-pyruvamide (580 mg), described by W. F. Gresham in U.S. Pat. No. 2,429,877, issued Oct. 28, 1947, 1.7 g of phosphorus pentoxide, 0.5 g of diatomaceous earth (Celite) in 75 ml of benzene is stirred at room temperature for 15 min. and then at 70° C for 11/2 hr. The reaction mixture is filtered. The filtrate is washed with water, dried (MgSO4) and concentrated to give the title compound, identical to the product of Example 15. at 70° C 2 hr The reaction mixture is filtered The filtrate is washed with water dried (MgSO4) concentrated

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

实验步骤: A mixture of 1-(o-hydroxyphenyl)pyrrole (500 mg), N,N-dimethyl-pyruvamide (580 mg), described by W. F. Gresham in U.S. Pat. No. 2,429,877, issued Oct. 28, 1947, 1.7 g of phosphorus pentoxide, 0.5 g of diatomaceous earth (Celite) in 75 ml of benzene is stirred at room temperature for 15 min. and then at 70° C for 11/2 hr. The reaction mixture is filtered. The filtrate is washed with water, dried (MgSO4) and concentrated to give the title compound, identical to the product of Example 15. at 70° C 2 hr The reaction mixture is filtered The filtrate is washed with water dried (MgSO4) concentrated

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: To a solution of N,N-dimethyl-2-oxopropanamide (413 mg, 3.59 mmol) in dry THF (10 mL) at 0° C. under an atmosphere of nitrogen was introduced ethynylmagnesium bromide (10 mL of a 0.5M solution in THF, 5.00 mmol) dropwise over 10 minutes. After warming to RT for 1 hr, water was introduced dropwise until gas evolution ceased and the resulting slurry concentrated in vacuo. The residue was slurried in DCM (50 mL) with sonication for 5 min. and the mixture filtered. Following re-suspension of the filter cake in water (10 mL), the pH was adjusted to 2 with 1M aqueous hydrochloric acid and the resulting hazy solution re-extracted with DCM (30 mL). The DCM extract was combined with the DCM filtrate, dried (Na2SO4), filtered and the filtrate concentrated in vacuo to furnish the crude title compound as a brown oil: 1H NMR (500 MHz, CDCl3) delta 1.68 (3H, s), 2.64 (1H, s), 3.08 (3H, s), 3.31 (3H, s), 5.25 (1H, br. s); LC-MS: m/z=+141.95 (M+H)+. the resulting slurry concentrated in vacuo The residue was slurried in DCM (50 mL) with sonication for 5 min. the mixture filtered re-suspension of the filter cake in water (10 mL) the resulting hazy solution re-extracted with DCM (30 mL) The DCM extract dried (Na2SO4) filtered the filtrate concentrated in vacuo

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

实验步骤: A mixture of 1-(o-hydroxyphenyl)pyrrole (500 mg), N,N-dimethyl-pyruvamide (580 mg), described by W. F. Gresham in U.S. Pat. No. 2,429,877, issued Oct. 28, 1947, 1.7 g of phosphorus pentoxide, 0.5 g of diatomaceous earth (Celite) in 75 ml of benzene is stirred at room temperature for 15 min. and then at 70° C for 11/2 hr. The reaction mixture is filtered. The filtrate is washed with water, dried (MgSO4) and concentrated to give the title compound, identical to the product of Example 15. at 70° C 2 hr The reaction mixture is filtered The filtrate is washed with water dried (MgSO4) concentrated