反应详情

温度

50 °C

A mixture of 1-bromo-3-nitromethyl-benzene (6.82 g, 31.6 mmol), formaline (35%, 5.22 ml, 66.3 mmol) and Et3N (2.2 ml, 15.78 mmol) was heated at 50° C. for 1 h, diluted with water and extracted with TBME. The organic phase was washed with brine, dried with MgSO4 and evaporated. The residue was crystallized from TBME/hexane to yield the title compound in the form of a colourless solid. TLC (hexane/EtOAc=2:1): Rf=0.2; HPLC: RtH2=3.117 min; 11H-NMR (400 MHz, CD3OD): 7.61-7.54 (m, 2H), 7.39-7.34 (m, 2H), 4.40 (d, 2H), 4.35 (d, 2H); MS: 298, 300 [(M+Na)+].

1. extractionextracted with TBME
2. washThe organic phase was washed with brine
3. dry with materialdried with MgSO4
4. customevaporated
5. customThe residue was crystallized from TBME/hexane