2-Bromoethanol → HCID 22036304, compound

5.00 g (45.82 mmol) of 3-hydroxy-6-methylpyridine are dissolved in 65 ml of dry DMF, 6.87 g (54.98 mmol) of 2-bromoethanol and 25.33 g (183.27 mmol) of potassium carbonate are added and the mixture is stirred at +150° C. for 8 h. The mixture is then filtered, and the filtrate is concentrated on a rotary evaporator. After addition of 100 ml of ethyl acetate and 30 ml of saturated aqueous sodium bicarbonate solution, the phases are separated and the aqueous phase is extracted two more times with in each case 30 ml of ethyl acetate. The combined organic phases are dried over magnesium sulphate, and the solvent is removed on a rotary evaporator. Without further purification, the residue is used for the subsequent reaction.

1. filtrationThe mixture is then filtered
2. concentrationthe filtrate is concentrated on a rotary evaporator
3. additionAfter addition of 100 ml of ethyl acetate and 30 ml of saturated aqueous sodium bicarbonate solution
4. customthe phases are separated
5. extractionthe aqueous phase is extracted two more times with in each case 30 ml of ethyl acetate
6. dry with materialThe combined organic phases are dried over magnesium sulphate
7. customthe solvent is removed on a rotary evaporator
8. customWithout further purification
9. customthe residue is used for the subsequent reaction

ORD record

ord-b9580af79e194ef48841109e877d7bc5

Source dataset

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08653109B2