Water → HCID 68646408, compound

Participants

Reaction Conditions

Reaction Steps

Of the compound from Example 160A, 243 mg (0.84 mmol) were introduced in 10 ml of acetonitrile under argon. Then at −15° C. 102 μl (1.17 mmol) of chlorosulphonyl isocyanate were added dropwise. After 30 min, the reaction solution was admixed with 20 ml of water and heated at 60° C. overnight. The reaction mixture was cooled and introduced into saturated aqueous sodium hydrogen carbonate solution. It was then extracted with ethyl acetate. The organic phase was dried over sodium sulphate, filtered and freed from the solvent on a rotary evaporator. The residue was taken up in 4 ml of dichloromethane and admixed with 4 ml of a 4M solution of hydrogen chloride in dioxane. A precipitate formed immediately. After a subsequent stirring time of 10 min, the batch was freed from the solvent on a rotary evaporator. Drying in an HV gave 219 mg (77% of theory) of the title compound in 79% purity.

Provenance & Evidence