Chlorosulfonyl isocyanate → HCID 54313059, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 0.16 ml of chlorosulphonyl isocyanate in 0.8 ml of methylene chloride is added dropwise at 0° C. to a solution of 0.69 g of [4-[6-(allyl-methyl-amino)-hexyloxy]-2-methylamino-phenyl]-(4-bromo-phenyl)-methanone in 4 ml of methylene chloride. After 3 hrs. at room temperature the mixture is again cooled to 0° C. and 0.8 ml of chlorosulphonyl isocyanate in 0.5 ml of methylene chloride is added dropwise. After 1 hr. at room temperature the mixture is worked-up with saturated sodium bicarbonate solution/methylene chloride and purified over silica gel with methylene chloride/methanol/25% aqueous ammonium hydroxide (95:5:0.5). There is obtained 0.26 g of 7-[6-(allyl-methyl-amino)-hexyloxy]-4-(4-bromo-phenyl)-1-methyl-1H-quinazolin-2-one, MS: m/e 484 (M+H+, 1 Br).

Provenance & Evidence