反应详情

温度

60 °C

A 2 L flask equipped with a stir bar was charged with DMSO (800 mL), K2CO3 (161 g, 1.6 mol) and 4-methoxy-2-fluoro-1-nitrobenzene (10 g, 0.58 mol). Mono-N-Boc-1,2-diaminoethane (94 g, 0.55 mol) was added to the reaction mixture and stirred for 12 h at 60° C. The reaction mixture was triturated with ice cold water (1.2 L) and the resulting yellow precipitate was collected by vacuum filtration. The precipitate washed several times with water (5×1 L) and dried on a high vacuum for 48 h to give the desired product as a bright yellow solid (178 g, 98%.)

1. customA 2 L flask equipped with a stir bar
2. customThe reaction mixture was triturated with ice cold water (1.2 L)
3. filtrationthe resulting yellow precipitate was collected by vacuum filtration
4. washThe precipitate washed several times with water (5×1 L)
5. customdried on a high vacuum for 48 h