Water → 4-Bromo-2,3-Dichlorophenol

Temperatur

10 °C

In a 250 mL round bottom flask 10 g of 2,3-dichlorophenol was dissolved in a solvent mixture of glacial acetic acid (16 mL) and chloroform (4 mL) and cooled to 10° C. To this was added bromine (3.45 mL) in 15 mL of glacial acetic acid dropwise while maintaining the temperature. The reaction was vigorously stirred while adding bromine and continued stirring vigorously 0.5 h after addition was finished. At this time reaction mixture was poured into a flask containing 60 mL of water and 30 mL of dichloromethane. Organic layer was separated and aqueous layer was extracted with dichloromethane (3×50 mL). The oraganic layers were combined and washed with Sat. sodium bicarbonate (3×100 mL) and brine (100 mL) and dried over sodium sulfate. The crude product (9.65 g) was carried in to the next step without any purification. 1H-NMR (400 MHz, CDCl3) δ: 7.47 and 6.89 (ABq, 2H), 5.69 (brs, 1H).

1. temperaturewhile maintaining the temperature
2. stirringcontinued stirring vigorously 0.5 h
3. additionafter addition
4. customAt this time reaction mixture
5. additionwas poured into a flask
6. customOrganic layer was separated
7. extractionaqueous layer was extracted with dichloromethane (3×50 mL)
8. washwashed with Sat. sodium bicarbonate (3×100 mL) and brine (100 mL)
9. dry with materialdried over sodium sulfate
10. customThe crude product (9.65 g) was carried in to the next step without any purification

ORD-Eintrag

ord-f9991c6d1c2e4e06a2d11f53d64c3957

Quelldatensatz

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08980950B2