4-bromo-2-fluoro-N-methylaniline synthesis
- Product Name:4-bromo-2-fluoro-N-methylaniline
- CAS Number:213190-12-6
- Molecular formula:C7H7BrFN
- Molecular Weight:204.04
Yield:213190-12-6 93%
Reaction Conditions:
Stage #1: formaldehyd;4-bromo-2-fluoroanilinewith sodium methylate in methanol; for 2 h;Reflux;
Stage #2: with methanol;sodium tetrahydroborate at 0; for 1 h;Reflux;
Steps:
Preparation of 4-bromo-2-fluoro-N-methylaniline (4).
At the room temperature to 100 ml with a magnetic stirring bar in a round-bottom flask by adding MeOH (26.0 ml), 3 (0.5g, 2 . 63mmol), NaOMe (0.71g, 13 . 16mmol) and low polyoxymethylene (0.394g, 13 . 16mmol). Reflux the reaction mixture 2 hours. Then the reaction mixture cooled to 0 °C, and to divide the NaHB 4 (0.5g, 13 . 16mmol). After the addition, the reaction mixture is reflux again 1 hour. After finishing the reaction, removal of MeOH, adding water (50 ml), and using EtOAc (3x30mL) extraction. The combined organic extract water (30 ml), brine (30 ml) washing, through MgSO 4 drying and vacuum concentration. Residue through silica gel (using EtOAc: hexane (0.5: 9.5) as eluant) to purification, the 4 (0.5g, 93%), as a brown oil.
References:
CN102985411,2016,B Location in patent:Paragraph 0394; 0397-0398
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