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4102-84-5

6-chloro-4-nitro-o-cresol synthesis

6synthesis methods
-

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