6-fluoro-1-benzofuran-3-one

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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

Conditions: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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

Conditions: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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