反应详情

温度

20 °C

To a 2 L three neck RB flask provided with a mechanical stirrer were charged a solution of 4′-chloro-5,5-dimethyl-3,4,5,6-tetrahydro-[1,1′-biphenyl]-2-carbaldehyde (50.0 g) in toluene (250 mL), BOC-piperazine (48.2 g) and anhydrous THF (250 mL). The yellow solution was stirred at 20° C. for 5 min. Sodium triacetoxyborohydride (52.7 g) was added in portion (note: the internal temperature rose to ˜29.5° C. in 15 min cooling may be needed). The yellow mixture was stirred at ˜25° C. for NLT 4 hrs. A conversion of starting material to product of 99.5% was observed by HPLC after a 3 hour reaction time.

1. waitthe internal temperature rose to ˜29.5° C. in 15 min
2. temperaturecooling may
3. stirringThe yellow mixture was stirred at ˜25° C. for NLT 4 hrs
4. waitA conversion of starting material to product of 99.5% was observed by HPLC after a 3 hour
5. customreaction time