2-甲基-4,6,7,8,9,9a-六氢-3H-吡嗪并[1,2-a]吡嗪-1-one

反应条件: temp:105.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of crude (+/−)-tert-butyl (3-bromo-2-chloro-5-cyanophenyl)carbamate (78 mg, 0.236 mmol), 2-methyloctahydro-1H-pyrazino[1,2-a]pyrazin-1-one (40 mg, 0.236 mmol), Pd2dba3 (21.65 mg, 0.024 mmol), BINAP (44.2 mg, 0.071 mmol) and Cs2CO3 (231 mg, 0.709 mmol) in Dioxane (2.5 mL) was evacuated and filled with nitrogen 3 times and heated at 105° C. for 8 h. LC-MS showed completion of reaction. The reaction mixture was filtered through a plug of Celite and the filtrate was concentrated. Purification via flash chromatography (0-5% MeOH in DCM, 12 g) gave (+/−)-tert-butyl (2-chloro-5-cyano-3-(8-methyl-9-oxohexahydro-1H-pyrazino[1,2-a]pyrazin-2(6H)-yl)phenyl)carbamate (60 mg) as a yellow oil. was evacuated filled with nitrogen 3 times completion of reaction The reaction mixture was filtered through a plug of Celite the filtrate was concentrated Purification via flash chromatography (0-5% MeOH in DCM, 12 g)

反应条件: temp:105.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of crude (+/−)-tert-butyl (3-bromo-2-chloro-5-cyanophenyl)carbamate (78 mg, 0.236 mmol), 2-methyloctahydro-1H-pyrazino[1,2-a]pyrazin-1-one (40 mg, 0.236 mmol), Pd2dba3 (21.65 mg, 0.024 mmol), BINAP (44.2 mg, 0.071 mmol) and Cs2CO3 (231 mg, 0.709 mmol) in Dioxane (2.5 mL) was evacuated and filled with nitrogen 3 times and heated at 105° C. for 8 h. LC-MS showed completion of reaction. The reaction mixture was filtered through a plug of Celite and the filtrate was concentrated. Purification via flash chromatography (0-5% MeOH in DCM, 12 g) gave (+/−)-tert-butyl (2-chloro-5-cyano-3-(8-methyl-9-oxohexahydro-1H-pyrazino[1,2-a]pyrazin-2(6H)-yl)phenyl)carbamate (60 mg) as a yellow oil. was evacuated filled with nitrogen 3 times completion of reaction The reaction mixture was filtered through a plug of Celite the filtrate was concentrated Purification via flash chromatography (0-5% MeOH in DCM, 12 g)

反应条件: temp:105.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of crude (+/−)-tert-butyl (3-bromo-2-chloro-5-cyanophenyl)carbamate (78 mg, 0.236 mmol), 2-methyloctahydro-1H-pyrazino[1,2-a]pyrazin-1-one (40 mg, 0.236 mmol), Pd2dba3 (21.65 mg, 0.024 mmol), BINAP (44.2 mg, 0.071 mmol) and Cs2CO3 (231 mg, 0.709 mmol) in Dioxane (2.5 mL) was evacuated and filled with nitrogen 3 times and heated at 105° C. for 8 h. LC-MS showed completion of reaction. The reaction mixture was filtered through a plug of Celite and the filtrate was concentrated. Purification via flash chromatography (0-5% MeOH in DCM, 12 g) gave (+/−)-tert-butyl (2-chloro-5-cyano-3-(8-methyl-9-oxohexahydro-1H-pyrazino[1,2-a]pyrazin-2(6H)-yl)phenyl)carbamate (60 mg) as a yellow oil. was evacuated filled with nitrogen 3 times completion of reaction The reaction mixture was filtered through a plug of Celite the filtrate was concentrated Purification via flash chromatography (0-5% MeOH in DCM, 12 g)