Dichloromethane → HCID 86641324, compound

Participants

Reaction Steps

Methanesulfonyl chloride (39 μL) was added dropwise to a mixture composed of di-tert-butyl {8-hydroxy-2-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-2,7,8,9-tetrahydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-4-yl}imidodicarbonate of Example 32 (240 mg), dehydrated dichloromethane (6 mL) and triethylamine (88 μL) under cooling in an ice bath. The ice bath was removed and the mixture was stirred for two hours. After confirming that the raw material disappeared, the reaction mixture was diluted with chloroform and washed with water. The organic layer was dried over anhydrous sodium sulfate and then filtered, and the filtrate was concentrated under reduced pressure. Dichloromethane and hexane were added to the residue, and the precipitated solid was collected by filtration to obtain the title compound (253 mg, 93%). The resulting compound was directly used for the next reaction without purification.

Provenance & Evidence