Ammonium Hydroxide → HCID 10606940, Verbindung

Crude 5-bromo-3-isopropoxypyridine (3.71 g, 17.18 mmol) was dissolved in methanol (46 mL) and added to concentrated ammonium hydroxide (29.7%, 14.8 M, 50 mL) and copper(I) bromide (2.46 g, 17.18 mmol) in a heavy-walled glass pressure-tube apparatus. The tube was sealed and the mixture was stirred and heated at 170° C. (oil bath temperature) for 24 h. After cooling, the solution was concentrated by rotary evaporation. Sodium carbonate solution (17.6%, 200 mL) was added, and the mixture was extracted with CH2Cl2 (4×50 mL). The combined CH2Cl2 extracts were dried (MgSO4), filtered, and concentrated by rotary evaporation to give 1.88 g (72.0%) of a brown oil.

1. customThe tube was sealed
2. temperatureAfter cooling
3. concentrationthe solution was concentrated by rotary evaporation
4. additionSodium carbonate solution (17.6%, 200 mL) was added
5. extractionthe mixture was extracted with CH2Cl2 (4×50 mL)
6. dry with materialThe combined CH2Cl2 extracts were dried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated by rotary evaporation

ORD-Eintrag

ord-5be74c21cef9416baf9b31bfdd3ca492

Quelldatensatz

uspto-grants-2003_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06627648B1