2,6-Dichloro-3,4-dimethylphenol synthesis
- Product Name:2,6-Dichloro-3,4-dimethylphenol
- CAS Number:1570-67-8
- Molecular formula:C8H8Cl2O
- Molecular Weight:191.05
95-65-8
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Yield:1570-67-8 25%
Reaction Conditions:
with sulfuryl dichloride in dichloromethane at 50; for 4 h;
Steps:
To a sol. of 3,4-dimethylphenol (3.00 g, 24.6 mmol) in CH2Cl2 (5 mL) was added SO2Cl2 (4.98 mL, 61.3 mmol). The resulting sol. was heated to 50 °C for 4 h. The mixture was poured onto ice-water. CH2CI2 (200 mL) was added, the layers were separated, and the org. layer was washed with water, then with aq. sat. NaHCO3. The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification by FC (EtOAc/heptane 1:4) yielded the title compound (1.174g , 25%). LC-MS: tR = 0.97 min. Rf = 0.38 (EtOAc/heptane 1:4).
References:
WO2006/21402,2006,A1 Location in patent:Page/Page column 39
1124-04-5
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