反应详情

Oxalyl chloride (40.9 ml) is added dropwise to a stirred solution of the benzocyclobutene carboxylic acid obtained in the previous step (90.2 g) dissolved in a mixture of DMF (3 ml) and methylene chloride (450 ml). The reaction mixture is stirred at RT overnight and added dropwise to an ice cold solution of piperidine (185 ml) in methylene chloride (450 ml) over a 90-minute period. The reaction mixture is allowed to stir at RT for five hours, washed with aqueous 5% hydrochloric acid, dried, filtered and evaporated affording the desired product as an oil, which is used in the next step without further purification.

1. customobtained in the previous step (90.2 g)
2. stirringto stir at RT for five hours
3. washwashed with aqueous 5% hydrochloric acid
4. customdried
5. filtrationfiltered
6. customevaporated