Potassium Carbonate → HCID 70651086, compound

Temperature

0 °C

2-amino-4-methyl-5-bromo-pyridine (3 g, 16 mmol) and K2CO3 (5.5 g, 40 mmol) were added into acetonitrile (35 mL), cooled to 0° C. on ice-salts cooling bath. 2-chloroethyl chloroformate (2.75 g, 19.2 mmol) was added dropwise, and after its completion, the mixture was raised to room temperature, agitated for 1 hr, and refluxed under heat for 3 hrs. TLC (petroleum ether/ethyl acetate=3:1) was employed to monitor the reaction. After the starting materials completely reacted, acetonitrile was removed by evaporation. The resulting mixture was diluted by adding dichloromethane (100 mL), washed sequentially with water and saturated saline solution, and dried over anhydrous sodium sulfate. Column chromatography afforded 2.6 g of white solid, yield 63%.

1. temperatureafter its completion, the mixture was raised to room temperature
2. temperaturerefluxed
3. temperatureunder heat for 3 hrs
4. customthe reaction
5. customAfter the starting materials completely reacted
6. customacetonitrile was removed by evaporation
7. additionThe resulting mixture was diluted
8. additionby adding dichloromethane (100 mL)
9. washwashed sequentially with water and saturated saline solution
10. dry with materialdried over anhydrous sodium sulfate

ORD record

ord-21016ad25ad24b0cb2e8f8f99e575af8

Source dataset

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09416144B2