Ammonia → HCID 21909291, compound

Temperature

100 °C

To a mixture of methyl 4-(4-ethylbenzyl)-3-hydroxy-benzoate (0.20 g) and 28% aqueous ammonia solution (6 mL) in ethanol (3 mL) was added ammonium chloride (0.079 g), and the mixture was stirred in sealed tube at 100° C. for 14 hours. The reaction mixture was concentrated under reduced pressure, water was added to the residue, and the resulting mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. A mixed solvent of dichloromethane and methanol (10:1) was added to the residue, and an insoluble material was collected by filtration and dried to give 4-(4-ethylbenzyl)-3-hydroxybenzamide (0.065 g).

1. concentrationThe reaction mixture was concentrated under reduced pressure, water
2. additionwas added to the residue
3. extractionthe resulting mixture was extracted with ethyl acetate
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. customthe solvent was removed under reduced pressure
6. additionA mixed solvent of dichloromethane and methanol (10:1) was added to the residue
7. filtrationan insoluble material was collected by filtration
8. customdried

ORD record

ord-cba0f3091fc047919fb8869dade91a53

Source dataset

uspto-grants-2006_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07129381B2