反应详情

To an ice-cold solution of 3-(4-methylpiperazine-1-carbonyl)-7-oxa-bicyclo[2,2,1]-heptane-2-carboxylic acid (938 mg, 3.5 mmole) in methylene chloride (30 mL) was added thionyl chloride (1 mL) followed by a few drops of DMF. After stirring at ice-cold temperature for 30 min, the ice-bath was removed and stirring continued at room temperature overnight. The excess thionyl chloride was removed using oil-free vacuum pump at −50° C. and to the residue was added methylene chloride (10 mL). The resulted thin slurry of 1 was used as such in the next reaction.

1. customthe ice-bath was removed
2. stirringstirring
3. waitcontinued at room temperature overnight
4. customThe excess thionyl chloride was removed
5. customat −50° C.
6. additionto the residue was added methylene chloride (10 mL)
7. customsuch in the next reaction