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ChemicalBook CAS DataBase List 2,6-DICHLORO-5-METHYL-1H-1,3-BENZODIAZOLE

2,6-DICHLORO-5-METHYL-1H-1,3-BENZODIAZOLE synthesis

2synthesis methods
683240-81-5 Synthesis
2H-Benzimidazol-2-one,5-chloro-1,3-dihydro-6-methyl-(9CI)

683240-81-5
20 suppliers
$225.00/1g

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Yield:683240-82-6 98%

Reaction Conditions:

with trichlorophosphate at 120; for 2 h;Product distribution / selectivity;a screw cap pressure tube;

Steps:

49.b

(b) Preparation of the intermediate compound 2,5-dichloro-6-methyl-lH-benzo[d]imidazole:To 5-chloro-6-methyl-lH-benzo[d]imidazol-2(3H)-one (0.25 g), phosphoryl trichloride (POCI3, 4 mL) was added, the reaction mixture was heated in a screw cap pressure tube at 12O0C for 2 hours and concentrated in vacuo. The residue was neutralized with sodium hydroxide, the resulting off-pale yellow solid was filtered, washed with water (3χ50 mL) and dried under high vacuum to give 0.27 g (98 % yield) of 2,5-dichloro-6-methyl-lH-benzo[d]imidazole

References:

WO2011/23812,2011,A1 Location in patent:Page/Page column 95