4-methyl-3-(methylamino)phenol synthesis
- Product Name:4-methyl-3-(methylamino)phenol
- CAS Number:6265-13-0
- Molecular formula:C8H11NO
- Molecular Weight:137.18
156267-11-7
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6265-13-0
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Yield:6265-13-0 59%
Reaction Conditions:
with hydrogen bromide;acetic acid in water at 110; for 5 h;
Steps:
4-methyl-3-(methylamino)phenol (21)
Compound 20 (0.9 g, 5.95 mmol) was dissolved in glacial AcOH (9 mL) at rt after which aqueous HBr (48%, 9 mL) was added. The resulting solution was heated at 110° C for 5 h before cooling. After which, the reaction mixture was diluted with 50 mL DI water, and the pH of the solution was adjusted to 5-6 with 2 M NaOH solution. The aqueous solution was extracted with DCM (3 x 50 mL). The combined organic layers were rinsed with brine, dried over anhydrous Na2S04. The solvent was removed using a rotary evaporator and the residue was purified by flash column chromatography with silica gel (30 g), using EtO Ac/Hexane as eluent to give compound 21
References:
WO2020/23911,2020,A2 Location in patent:Page/Page column 50
50868-72-9
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6265-13-0
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