1-[2-(吗啉-4-基甲基)苯基]甲胺

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

实验步骤: A mixture 6-bromo-4-chloro-2H-phthalazin-1-one (150 mg, 0.58 mmol), 2-morpholin-4-ylmethyl-benzylamine (132 mg, 0.64 mmol), Pd2(dba)3 (53 mg, 0.058 mmol), rac-BINAP (132 mg, 0.17 mmol) and NaOt-Bu (140 mg, 1.45 mmol) in DMA (6 mL) was heated at 80° C. for 1 h. The mixture was allowed to cool, diluted with EtOAc (25 mL) and washed with water (25 mL). The organic layer was dried over anhydrous sodium sulfate and concentrated. Chromatography on silica (EtOAc/hexanes) yielded the title compound. 4-Chloro-6-(2-morpholin-4-ylmethyl-benzylamino)-2H-phthalazin-1-one: 52 mg (23.3%): m/z (M+H)=385. 1H-NMR (DMSO-d6) δ: 12.27 (s, 1H), 7.85 (d, 1H), 7.51 (m, 1H), 7.22 (m, 2H), 7.16 (m, 2H), 7.11 (dd, 1H), 6.73 (s, 1H), 4.55 (d, 2H), 3.50 (m, 6H), 2.23 (m, 4H). to cool washed with water (25 mL) The organic layer was dried over anhydrous sodium sulfate concentrated

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

实验步骤: A mixture 6-bromo-4-chloro-2H-phthalazin-1-one (150 mg, 0.58 mmol), 2-morpholin-4-ylmethyl-benzylamine (132 mg, 0.64 mmol), Pd2(dba)3 (53 mg, 0.058 mmol), rac-BINAP (132 mg, 0.17 mmol) and NaOt-Bu (140 mg, 1.45 mmol) in DMA (6 mL) was heated at 80° C. for 1 h. The mixture was allowed to cool, diluted with EtOAc (25 mL) and washed with water (25 mL). The organic layer was dried over anhydrous sodium sulfate and concentrated. Chromatography on silica (EtOAc/hexanes) yielded the title compound. 4-Chloro-6-(2-morpholin-4-ylmethyl-benzylamino)-2H-phthalazin-1-one: 52 mg (23.3%): m/z (M+H)=385. 1H-NMR (DMSO-d6) δ: 12.27 (s, 1H), 7.85 (d, 1H), 7.51 (m, 1H), 7.22 (m, 2H), 7.16 (m, 2H), 7.11 (dd, 1H), 6.73 (s, 1H), 4.55 (d, 2H), 3.50 (m, 6H), 2.23 (m, 4H). to cool washed with water (25 mL) The organic layer was dried over anhydrous sodium sulfate concentrated