Bromine → 3-Bromo-6-methoxy-2-methylpyridine

2-Methoxy-6-methylpyridine (10 mL, 81 mmol) was suspended in a 0.15 mol//L disodium hydrogen phosphate aqueous solution (160 mL). Thereafter, a solution prepared by suspending bromine (4.15 mL, 81 mmol) in a 0.15 mol//L disodium hydrogen phosphate aqueous solution (160 mL) was added dropwise to the suspension at room temperature over 1 hour. The reaction solution was stirred at the same temperature as described above overnight. Thereafter, the reaction solution was extracted with methylene chloride (300 mL) three times. Organic layers were gathered. The resultant was dried over anhydrous magnesium sulfate and was then filtrated, followed by vacuum concentration. The obtained residue was distilled away under reduced pressure (91° C.-96° C./16 mmHg), so as to obtain 9.47 g of 3-bromo-6-methoxy-2-methyl-pyridine.

1. customThereafter, a solution prepared
2. additionwas added dropwise to the suspension at room temperature over 1 hour
3. waitas described above overnight
4. extractionThereafter, the reaction solution was extracted with methylene chloride (300 mL) three times
5. dry with materialThe resultant was dried over anhydrous magnesium sulfate
6. filtrationwas then filtrated
7. concentrationfollowed by vacuum concentration
8. distillationThe obtained residue was distilled away under reduced pressure (91° C.-96° C./16 mmHg)

ORD record

ord-59007b2429d34e4c89a5bfcaa39d3b20

Source dataset

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09018238B2