Acetic Acid → 2,4,6-Triethylbenzyl bromide

Temperature

45 °C

To a mixture of 3.00 g of 1,3,5-triethylbenzene (purity: 93%) and 5.58 g of acetic acid, 0.82 g of paraformaldehyde and 4.7 mL of a 33% solution of hydrogen bromide in acetic acid were added. This mixture was heated at 45° C. for 7.5 hours under stirring. After the reaction mixture was cooled to room temperature, 16.8 g of water and 16.8 g of toluene were added thereto. The reaction mixture was separated. The organic layer was washed sequentially with 11.2 g of water, a mixture of 5.6 g of an aqueous saturated sodium hydrogen carbonate solution and 5.6 g of water, and 11.2 g of water, dried over anhydrous magnesium sulfate, and then concentrated to obtain 4.72 g of 2,4,6-triethylbenzyl bromide (GC-area: 84%) as a yellow oil.

1. additionwere added
2. temperatureAfter the reaction mixture was cooled to room temperature
3. customThe reaction mixture was separated
4. washThe organic layer was washed sequentially with 11.2 g of water
5. additiona mixture of 5.6 g of an aqueous saturated sodium hydrogen carbonate solution and 5.6 g of water, and 11.2 g of water
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated

ORD record

ord-dce1f1f1881a41c7a16c0d619a96225d

Source dataset

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08507410B2