Methylamine → HCID 9834124, compound

Temperature

100 °C

Crude 3-bromo-1-(3-pyridyloxy)butane (2.00 g, 8.69 mmol) from the previous step was dissolved in methanol (10 mL) and added to a 40 wt % aqueous solution of methylamine (30 mL) in a heavy-walled glass pressure-tube apparatus. The mixture was stirred and heated at 100° C. (oil bath temperature) for 16 h. After cooling, the mixture was concentrated by rotary evaporation, and the product was extracted with chloroform (4×50 mL). The combined chloroform extracts were dried (Na2SO4), filtered and concentrated by rotary evaporation to give 1.25 g of a pale-yellow oil. Purification by vacuum distillation yielded 0.94 g (60.3%) of a colorless oil, bp 65-67° C. at 0.5 mm Hg.

1. temperatureAfter cooling
2. concentrationthe mixture was concentrated by rotary evaporation
3. extractionthe product was extracted with chloroform (4×50 mL)
4. dry with materialThe combined chloroform extracts were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated by rotary evaporation

ORD record

ord-9c13082ffbdb490c8797562234683c7a

Source dataset

uspto-grants-2003_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06627648B1