6-甲氧基-3-苯并呋喃酮

反应条件: temp:0.00; pressure:0.00; stir:

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 Example 1109B (0.152 g) and 1-methylpiperazine (0.22 g) in DMSO (1 ml) was heated at 150 C for 30 min, allowed to cool to r.t. (room temperature) then partitioned between water and EtOAc. Organics were dried (Na2SO4), concentrated and purified via silica gel chromatography eluting with 5% MeOH-CH2Cl2 to give the title compound. MS ESI(+)m/e 233.0(M+H)+. then partitioned between water and EtOAc Organics were dried (Na2SO4) concentrated purified via silica gel chromatography eluting with 5% MeOH-CH2Cl2

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

实验步骤: CsCO3 (5.36 g) was added in portions over 10 min to an ice cold solution of Example 1109A (3.2 g) in DMF (140 mL). The resulting mixture was stirred for 30 min then diluted with water and extracted with ether (3×). the combined extracts were dried (Na2SO4), and concentrated to give 1.6 g of the title compound. MS ESI(−) m/e 151.1 (M−H)−. extracted with ether (3×) the combined extracts were dried (Na2SO4) concentrated

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

实验步骤: A mixture of Example 1109B (0.152 g) and 1-methylpiperazine (0.22 g) in DMSO (1 ml) was heated at 150 C for 30 min, allowed to cool to r.t. (room temperature) then partitioned between water and EtOAc. Organics were dried (Na2SO4), concentrated and purified via silica gel chromatography eluting with 5% MeOH-CH2Cl2 to give the title compound. MS ESI(+)m/e 233.0(M+H)+. then partitioned between water and EtOAc Organics were dried (Na2SO4) concentrated purified via silica gel chromatography eluting with 5% MeOH-CH2Cl2

反应条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 6-fluoro-benzofuran-3-one (CAS 351528-80-8) (5.93 g, 39 mmol), sodium acetate (6.587 g, 80 mmol) and hydroxylamine hydrochloride (5.553 g, 80 mmol) in ethanol (70 ml) was refluxed for 4 h. Cooled to 23° C., filtered the precipitate off, washed with aqueous ethanol and dried in high vacuum to give the title compound as a white solid (5.19 g, 80%, HPLC 1.489 min); MS (ISN) m/e=168.1 [(M−H)−]. was refluxed for 4 h filtered the precipitate off, washed with aqueous ethanol dried in high vacuum

反应条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 6-fluoro-benzofuran-3-one (CAS 351528-80-8) (5.93 g, 39 mmol), sodium acetate (6.587 g, 80 mmol) and hydroxylamine hydrochloride (5.553 g, 80 mmol) in ethanol (70 ml) was refluxed for 4 h. Cooled to 23° C., filtered the precipitate off, washed with aqueous ethanol and dried in high vacuum to give the title compound as a white solid (5.19 g, 80%, HPLC 1.489 min); MS (ISN) m/e=168.1 [(M−H)−]. was refluxed for 4 h filtered the precipitate off, washed with aqueous ethanol dried in high vacuum