N1,N1,2,6-TETRAMETHYL-4-BROMOANILINE synthesis
- Product Name:N1,N1,2,6-TETRAMETHYL-4-BROMOANILINE
- CAS Number:50638-54-5
- Molecular formula:C10H14BrN
- Molecular Weight:228.13
50-00-0
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$10.00/25g
64-18-6
1126 suppliers
$22.12/250ML
24596-19-8
340 suppliers
$8.00/10g
50638-54-5
37 suppliers
$92.79/1g
Yield:50638-54-5 91%
Reaction Conditions:
Stage #1: formaldehyd;formic acid;4-bromo-2,6-dimethylphenylamine in water at 23; for 2 h;Heating / reflux;
Stage #2: with sodium hydrogencarbonate in water;
Steps:
2 4-bromo-N,N,2,6-tetramethylaniline
Reference Example 2 4-bromo-N,N,2,6-tetramethylaniline To a solution of 4-bromo-2,6-dimethylaniline (50 g, 0.250 moL) and formic acid (375 g, 32.6 equivalents) was added 37% formaldehyde (50.7 g, 2.5 equivalents) at 23°C, and the mixture was stirred under refluxing for 2 hr. The solvent was evaporated under reduced pressure. Ethyl acetate (200 mL) and 5% aqueous sodium hydrogen carbonate solution (500 mL) were added to the residue, and the mixture was partitioned. The organic layer was successively washed with water (100 mL) and 5% aqueous sodium hydrogen carbonate solution (100 mL). The organic layer was dried over anhydrous magnesium sulfate, and the mixture was filtered naturally. The filtrate was concentrated under reduced pressure and the residue was distilled under reduced pressure to give the title compound (52.0 g, colorless liquid). yield 91%. 1H-NMR (300MHz, CDCl3, TMS) δ: 2.26 (s, 6H), 2.79 (s, 6H), 7.12 (s, 2H).
References:
EP1927596,2008,A1 Location in patent:Page/Page column 20-21
50-00-0
893 suppliers
$10.00/25g
24596-19-8
340 suppliers
$8.00/10g
50638-54-5
37 suppliers
$92.79/1g