Hydrochloric Acid → 1,4-Bis[4-[(1-benzyloxyureido)methyl]phenoxy]butane

Temperatur

80 °C

60% Sodium hydride (0.41 g) and 1.71 g of benzyloxyurea were added to 20 ml of dimethylformamide and the mixture was stirred at 80° C. for 7.5 hours. 1,4-Bis(4-chloromethylphenoxy)butane (1.74 g) was added to the reaction mixture at room temperature and the mixture was stirred at 95° C. for 0.5 hour. The reaction product was cooled to room temperature, poured into ice water, mixed with 1N hydrochloric acid and then extracted with ethyl acetate. The organic layer was washed with water and saturated sodium chloride aqueous solution in that order and dried over anhydrous magnesium sulfate and then the solvent was evaporated under a reduced pressure. The resulting crude product was washed with ethyl acetate to obtain 1.94 g of 1,4-bis[4-[(1-benzyloxyureido)methyl]phenoxy]butane.

1. stirringthe mixture was stirred at 95° C. for 0.5 hour
2. temperatureThe reaction product was cooled to room temperature
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with water and saturated sodium chloride aqueous solution in that order
5. dry with materialdried over anhydrous magnesium sulfate
6. customthe solvent was evaporated under a reduced pressure
7. washThe resulting crude product was washed with ethyl acetate

ORD-Eintrag

ord-b6ddbc7cf4a0424f8ca1050d7058a9e0

Quelldatensatz

uspto-grants-1997_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05643931