Water → HCID 10719654, compound

Participants

Reaction Steps

7 g (217.3 mmol) of N-(2-fluoro-4-aminophenyl)-N-benzyl amine (4) obtained from the aforesaid process was dissolved in 500 mL dichloromethane, then 60 g (434.6 mmol) of K2CO3 was added thereto, with stirring in an ice bath for 10 minutes. 92 mL (652 mmol) Cbz-Cl was dropped slowly to the mixture over 1 hour and then the mixture was warmed to room temperature. After completion of the reaction, 200 mL water was added to the reaction solution under stirring for 1 hour. The resultant mixture was allowed to stand for separation, and the dichloromethane layer was washed in sequence with 10% diluted hydrochloric acid and NaHCO3 solution. The obtained dichloromethane layer was rotary evaporated to afford a light yellow oil, which was purified with column chromatography to obtain 80 g of a white solid, with a yield of 76.2%.

Provenance & Evidence