反応 #92817

反応方程式

2,6-diisopropylaniline

1-bromopyrrolidine-2,5-dione

water

→

4-bromo-2,6-diisopropylaniline

収率 97.0%

溶媒

DMF

DMF

反応条件

後処理

1. 1
   workup.ADDITIONAfter addition
2. 2
   その他reaction mixture
3. 3
   workup.ADDITIONThe reaction mixture was poured into 500 ml
4. 4
   抽出extracted with 3×150 ml ether
5. 5
   洗浄The combined extracts were washed with 150 ml
6. 6
   乾燥dried over MgSO4
7. 7
   その他evaporated to dryness
8. 8
   workup.DISTILLATIONThe residue was purified by vacuum distillation

実験手順

A three neck round bottom flask was charged with 2,6-diisopropylaniline (22.96 g, 130 mmol) and DMF (Volume: 250 ml). A solution of 1-bromopyrrolidine-2,5-dione (23.05 g, 130 mmol) in 100 ml DMF was added into reaction mixture drop wise at 0° C. After addition was over; reaction mixture was stirred for 2 days at room temperature. The reaction mixture was poured into 500 ml deionized water and extracted with 3×150 ml ether. The combined extracts were washed with 150 ml deionized water, 150 ml 10% lithium chloride, dried over MgSO4 and evaporated to dryness. The residue was purified by vacuum distillation to yield 4-bromo-2,6-diisopropylaniline (32.3 g; 97%).

出典