反应详情

A sample of tert-butyl 4-(2-(4-chloro-2-ureidophenoxy)acetyl)piperidine-1-carboxylate (264 mg, 0.64 mmol) was dissolved in CH2Cl2 (8 mL) and TFA (4 mL). The resultant homogeneous solution was stirred for 3 h and concentrated in vacuo. The resultant residue was partitioned between EtOAc and sat. NaHCO3. The phases were separated and the aqueous phase was basified to pH˜14 (paper) with 1N NaOH before being extracted with EtOAc (twice). The organic extracts were combined, washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo to afford 1-(5-chloro-2-(2-oxo-2-(piperidin-4-yl)ethoxy)phenyl)urea. LC/MS [M+H]+=312.07, [M+Na]+=334.04.

1. concentrationconcentrated in vacuo
2. customThe resultant residue was partitioned between EtOAc and sat. NaHCO3
3. customThe phases were separated
4. extractionbefore being extracted with EtOAc (twice)
5. washwashed with brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo