反应详情

To an ice-cooled solution of 9-(3,4-dichloro-phenylamino)-3-aza-spiro[5.5]undecane-3-carboxylic acid tert-butyl ester (258 mg, 0.624 mmol) in dichloromethane (10 mL) a solution of trifluoroacetic acid (4 mL) in dichloromethane (5 mL) was added. The mixture was stirred a room temperature over night. Water was added followed by sodium hydroxide 3 M to pH 9-10. The aqueous layer was extracted with dichloromethane (4×40 mL). The combined organic layers were washed with brine, dried with sodium sulphate and evaporated to give (3-aza-spiro[5.5]undec-9-yl)-(3,4-dichloro-phenyl)-amine (164 mg 84%) as a brownish solid. Mp. 128-132° C.

1. additionwas added
2. extractionThe aqueous layer was extracted with dichloromethane (4×40 mL)
3. washThe combined organic layers were washed with brine
4. dry with materialdried with sodium sulphate
5. customevaporated