反応 #85836

反応方程式

NaOH

HBr

tert-butyl 4-(4-amino-2-fluorophenyl)piperazine-1-carboxylate

NaNO2

HBr

→

1-(4-bromo-2-fluorophenyl)piperazine

溶媒

H2O

反応条件

後処理

1. 1
   温度The reaction was heated to 60° C.
2. 2
   workup.STIRRINGstirred for 2 hours
3. 3
   温度After cooling
4. 4
   抽出extracted with EA
5. 5
   洗浄washed with H2O and brine
6. 6
   その他dried
7. 7
   濃縮concentrated
8. 8
   その他to give black solid

実験手順

To a solution of tert-butyl 4-(4-amino-2-fluorophenyl)piperazine-1-carboxylate (885 mg, 3 mmol) in 8 mL of aq HBr was added a solution of NaNO2 (228 mg, 3.3 mmol) in 2 mL of H2O at 0° C., then the mixture was stirred at 0° C. for 40 minutes. After that, the mixture was poured into a solution of CuBr (905 mg, 6.3 mmol) in 8 mL aq HBr at 0° C. The reaction was heated to 60° C. and stirred for 2 hours. After cooling, the mixture was based with 2M NaOH to pH=8-9 and extracted with EA, washed with H2O and brine, dried and concentrated to give black solid. MS (m/z): 261 (M+H)+

出典