Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 22989699 | HCID 22989699 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 9834124 | HCID 9834124 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06627648B1 |
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| Source dataset | uspto-grants-2003_09 |
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| ORD ID | ord-9c13082ffbdb490c8797562234683c7a |
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| Source note | uspto-grants-2003_09 |
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