1,3-Benzodioxole → 1-Bromo-3,4-(methylenedioxy)benzene

Temperature

25 °C

A mixture of ceric ammonium nitrate (9.88 g, 18.0 mmol) and lithium bromide (1.5 g, 18.0 mmol) in acetonitrile (20 mL) was stirred for 30 minutes at 25° C. under nitrogen atmosphere. A solution of benzo[1,3]dioxol (2 g, 16 mmol) in acetonitrile (20 mL) was added slowly to it and the mixture was stirred for 4 hours at 25° C. The mixture was then diluted with water (50 mL) and extracted with ethyl acetate (3×50 mL). The organic layers were collected, combined, washed with water (50 mL), dried over anhydrous sodium sulphate, and concentrated under vacuum to give the desired product.

1. stirringthe mixture was stirred for 4 hours at 25° C
2. extractionextracted with ethyl acetate (3×50 mL)
3. customThe organic layers were collected
4. washwashed with water (50 mL)
5. dry with materialdried over anhydrous sodium sulphate
6. concentrationconcentrated under vacuum

ORD record

ord-1a28b934bcd84d12bac9f20b610b4af7

Source dataset

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07820654B2