6-chloro-4-nitro-o-cresol synthesis
- Product Name:6-chloro-4-nitro-o-cresol
- CAS Number:4102-84-5
- Molecular formula:C7H6ClNO3
- Molecular Weight:187.58
99-53-6
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Yield:4102-84-5 80%
Reaction Conditions:
with sulfuryl dichloride in acetic acid; for 16 h;Heating;Inert atmosphere;
Steps:
50.4 Step 4: Example 50g
To a solution of Example 50f (20.0 g, 130.7 mmol) in AcOH (600 mL) was added S02Cl2 (35.3 g, 261.4 mmol), the mixture was stirred at 70°C for 16 h under nitrogen atmosphere. Excess AcOH was removed in vacuo, followed by adding water slowly at 0°C with stirring. The precipitate was collected by filtration. The solid was dried under vacuum, treated with mixed solution (300 mL, Petroleum (1203) Ether/EtOAc = 20/1), stirred for 30 min and filtered to give the pure desired product Example 50g (19.5 g, yield 80%) as a yellow solid. (1204) LCMS [M+l]+ =188.0
References:
WO2019/240938,2019,A1 Location in patent:Paragraph 00451; 00454
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