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ChemicalBook CAS DataBase List 1,3-dibromo-2-chloro-5-methylbenzene

1,3-dibromo-2-chloro-5-methylbenzene synthesis

2synthesis methods
-

Yield:202925-05-1 55.3 %

Reaction Conditions:

with tert.-butylnitrite in ethanol at 25 - 50;Inert atmosphere;

Steps:

21

At 25°C and nitrogen atmosphere, tert-butyl nitrite (3.91 g, 33.4 mmol) was slowly added dropwise to ethanol (30 mL) solution with compound 21a (4.00 g, 13.4 mmol) dissolved. The reaction solution was stirred for 2 hours at 50 °C . The reaction solution was concentrated after being cooled down. The resulting residue was separated by silica gel column chromatography to obtain white solid 21b (2.1 g, yield: 55.3%). 1H NMR (500 MHz, Chloroform-d) δ 7.41 (s, 2H), 2.29 (s, 3H).

References:

EP4083032,2022,A1 Location in patent:Paragraph 0273; 0275