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(4aS,8aR)-4-(3,4-dimethoxyphenyl)-2-(piperidin-4-yl)-4a,5,6,7,8,8a-hexahydrophthalazin-1(2H)-one hydrochloride[ No CAS ]
[ 1416468-72-8 ]
Yield
Reaction Conditions
Operation in experiment
With 1-[(1-(cyano-?2-?ethoxy-?2-?oxoethylidenaminooxy)?dimethylamino-?morpholino)]-uronium hexafluorophosphate; N-ethyl-N,N-diisopropylamine; In dichloromethane; at 20.0℃; for 3.0h;
B42. tert-Butyl [(2R)-3-(3,5-difluorophenyl)-1 -{4-[(4aS,8aR)-4-(3,4-dimethoxyphenyl)-1 -oxo- 4a,5,6,7,8,8a-hexahydrophthalazin-2(1 H)-yl]piperidin-1 -yl}-1 -oxopropan-2-yl]carbamate; To a mixture of <strong>[205445-53-0]N-(tert-butoxycarbonyl)-3,5-difluoro-D-phenylalanine</strong> (500 mg) and DIPEA (1.08 ml) in DCM (15 ml) was added (4aS,8aR)-4-(3,4-dimethoxyphenyl)-2-(piperidin-4-yl)-4a,5,6,7,8,8a- hexahydrophthalazin-1 (2H)-one hydrochloride (677 mg; compound B76) and COMU (782 mg) and the reaction mixture was stirred for 3 h at RT. Afterwards a half -saturated aqueous sodium bicarbonate solution was added and the mixture was extracted twice with DCM. The combined organic phases were dried over magnesium sulphate and the organic layer was concentrated under reduced pressure. The resulting residue was purified by flash column chromatography [silica gel, eluent: Toluene/EtOAc, 9/1 (v/v)] to give the title compound as a solid.MS: calc: (654.74) found: [MH+] = 655.0; [MNa+] = 677.1 ; [MH+ - Boc] = 555.2
With 1-[(1-(cyano-?2-?ethoxy-?2-?oxoethylidenaminooxy)?dimethylamino-?morpholino)]-uronium hexafluorophosphate; N-ethyl-N,N-diisopropylamine; In dichloromethane; at 20.0℃; for 3.0h;
To a mixture of <strong>[205445-53-0]N-(tert-butoxycarbonyl)-3,5-difluoro-D-phenylalanine</strong> (500 mg) and DIPEA (1.08 ml) in DCM (15 ml) was added (4aS,8aR)-4-(3,4-dimethoxyphenyl)-2-(piperidin-4-yl)-4a,5,6,7,8,8a-hexahydrophthalazin-1(2H)-one hydrochloride (677 mg; compound B76) and COMU (782 mg) and the reaction mixture was stirred for 3 h at RT. Afterwards a half-saturated aqueous sodium bicarbonate solution was added and the mixture was extracted twice with DCM. The combined organic phases were dried over magnesium sulphate and the organic layer was concentrated under reduced pressure. The resulting residue was purified by flash column chromatography [silica gel, eluent: Toluene/EtOAc, 9/1 (v/v)] to give the title compound as a solid. [0560] MS: calc.: C35H44F2N4O6 (654.74) found: [MH+]=655.0; [MNa+]=677.1; [MH+-Boc]=555.2
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