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ChemicalBook CAS DataBase List 1H-Benzimidazole,2-chloro-5-methyl-(9CI)
4887-94-9

1H-Benzimidazole,2-chloro-5-methyl-(9CI) synthesis

2synthesis methods
-

Yield:4887-94-9 64%

Reaction Conditions:

with trichlorophosphate at 90; for 3 h;

Steps:

1.2 (2) 2-chloro-5-methyl-1H-benzo [d] imidazole

5-methyl-1,3-dihydrobenzimidazol-2-one (17.3 g, 116 mmol) andA mixture of phosphorous oxychloride (108 mL, 1.16 mol) was stirred at 90 ° C. for 3 hours. Cool to ambient temperatureAfter that, the reaction mixture was carefully added to chloroform (100 mL) and the resultingI collected it. The precipitate is saturated with NaHCO3 aq. Add to a mixture of (50 mL) and ethyl acetate (50 mL)Added. The separated organic phase was washed with water and brine and dried over MgSO4. After filtration, the filtrateDistilled under reduced pressure. The resulting precipitate is collected by filtration and washed successfully with isopropyl etherPurification gave the title compound (12.4 g, 64%).

References:

JP2019/52096,2019,A Location in patent:Paragraph 0115; 0117; 0118; 0119

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