3-hex-2-enyloxolane-2,5-dione

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A stirred mixture of 4-(3-amino-4-fluorobenzyl)-2H-phthalazin-1-one (0.1 g, 0.37 mmol; prepared in a manner similar to that described in Example 23), 3-hex-2-enyldihydrofuran-2,5-dione (0.068 g, 0.37 mmol) and toluene (10 ml) was heated under reflux for 20 hours, then the resulting solid was collected by filtration from the hot mixture, washed with ethyl acetate (3 ml) and dried in vacuo to give 2-{[2-fluoro-5-(4-oxo-3,4-dihydrophthalazin-1-ylmethyl)phenylcarbamoyl]methyl}oct-4-enoic acid (0.061 g) as an off-white solid, m.pt. 179–181° C.; 250 MHz 1H-nmr (d6-DMSO) δ (ppm): 0.7–0.9 (t, 3H) (CH3), 1.1–1.35 (m, 2H) (—CH2CH3), 1.75–2.0 (m, 2H) (—CH2CH2CH3), 2.0–2.3 (m, 2H) (—CH2CH═CH—), 2.3–2.8 (2×m obscured by DMSO signal, 2H+1H) (—CH2CH(CO2H)CH2—), 4.2 (s, 2H) (ArCH2—), 5.15–5.5 (m, 2H) (—CH═CH—) 6.9–7.2 (m, 2H) (2×ArH), 7.65–8.0 (m, 4H) (4×ArH), 8.2 (d, 1H) (ArH), 12.1 (br s, 1H) (CO2H), 12.6 (s, 1H) (CONH); m/z (M+H)+. 452, 93.7% purity. prepared in a manner similar to was heated under reflux for 20 hours the resulting solid was collected by filtration from the hot mixture washed with ethyl acetate (3 ml) dried in vacuo

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

実験手順: A stirred mixture of 4-(3-amino-4-fluorobenzyl)-2H-phthalazin-1-one (0.1 g, 0.37 mmol; prepared in a manner similar to that described in Example 23), 3-hex-2-enyldihydrofuran-2,5-dione (0.068 g, 0.37 mmol) and toluene (10 ml) was heated under reflux for 20 hours, then the resulting solid was collected by filtration from the hot mixture, washed with ethyl acetate (3 ml) and dried in vacuo to give 2-{[2-fluoro-5-(4-oxo-3,4-dihydrophthalazin-1-ylmethyl)phenylcarbamoyl]methyl}oct-4-enoic acid (0.061 g) as an off-white solid, m.pt. 179–181° C.; 250 MHz 1H-nmr (d6-DMSO) δ (ppm): 0.7–0.9 (t, 3H) (CH3), 1.1–1.35 (m, 2H) (—CH2CH3), 1.75–2.0 (m, 2H) (—CH2CH2CH3), 2.0–2.3 (m, 2H) (—CH2CH═CH—), 2.3–2.8 (2×m obscured by DMSO signal, 2H+1H) (—CH2CH(CO2H)CH2—), 4.2 (s, 2H) (ArCH2—), 5.15–5.5 (m, 2H) (—CH═CH—) 6.9–7.2 (m, 2H) (2×ArH), 7.65–8.0 (m, 4H) (4×ArH), 8.2 (d, 1H) (ArH), 12.1 (br s, 1H) (CO2H), 12.6 (s, 1H) (CONH); m/z (M+H)+. 452, 93.7% purity. prepared in a manner similar to was heated under reflux for 20 hours the resulting solid was collected by filtration from the hot mixture washed with ethyl acetate (3 ml) dried in vacuo

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A stirred mixture of 4-(3-amino-4-fluorobenzyl)-2H-phthalazin-1-one (0.1 g, 0.37 mmol; prepared in a manner similar to that described in Example 23), 3-hex-2-enyldihydrofuran-2,5-dione (0.068 g, 0.37 mmol) and toluene (10 ml) was heated under reflux for 20 hours, then the resulting solid was collected by filtration from the hot mixture, washed with ethyl acetate (3 ml) and dried in vacuo to give 2-{[2-fluoro-5-(4-oxo-3,4-dihydrophthalazin-1-ylmethyl)phenylcarbamoyl]methyl}oct-4-enoic acid (0.061 g) as an off-white solid, m.pt. 179–181° C.; 250 MHz 1H-nmr (d6-DMSO) δ (ppm): 0.7–0.9 (t, 3H) (CH3), 1.1–1.35 (m, 2H) (—CH2CH3), 1.75–2.0 (m, 2H) (—CH2CH2CH3), 2.0–2.3 (m, 2H) (—CH2CH═CH—), 2.3–2.8 (2×m obscured by DMSO signal, 2H+1H) (—CH2CH(CO2H)CH2—), 4.2 (s, 2H) (ArCH2—), 5.15–5.5 (m, 2H) (—CH═CH—) 6.9–7.2 (m, 2H) (2×ArH), 7.65–8.0 (m, 4H) (4×ArH), 8.2 (d, 1H) (ArH), 12.1 (br s, 1H) (CO2H), 12.6 (s, 1H) (CONH); m/z (M+H)+. 452, 93.7% purity. prepared in a manner similar to was heated under reflux for 20 hours the resulting solid was collected by filtration from the hot mixture washed with ethyl acetate (3 ml) dried in vacuo