4-Bromophenol → 2-[(4-Bromophenoxy)methyl]-2-methyloxirane

4-Bromophenol (80 g, 462 mmol), 2-(chloromethyl)-2-methyloxirane (400 ml) and potassium carbonate (95.86 g, 693 mmol) were mixed and allowed to react at 100° C. for 4 hours. After the reaction was completed, the mixture was concentrated under reduced pressure. Ethyl acetate (200 ml) and water (400 ml) were added thereto, followed by extraction. The water layer was extracted with ethyl acetate (200 ml). The organic layer was washed with water (200 ml) twice. The organic layer was then concentrated under reduced pressure to remove the ethyl acetate. Thereafter, toluene was added and the resulting mixture was concentrated under reduced pressure, obtaining 120 g of crude product.

1. customto react at 100° C. for 4 hours
2. concentrationthe mixture was concentrated under reduced pressure
3. additionEthyl acetate (200 ml) and water (400 ml) were added
4. extractionfollowed by extraction
5. extractionThe water layer was extracted with ethyl acetate (200 ml)
6. washThe organic layer was washed with water (200 ml) twice
7. concentrationThe organic layer was then concentrated under reduced pressure
8. customto remove the ethyl acetate
9. additionThereafter, toluene was added
10. concentrationthe resulting mixture was concentrated under reduced pressure

ORD record

ord-023e6a7af9ab4b9580fc9acc9b99ab86

Source dataset

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08598358B2