HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Methoxypropylamine → HCID 178495257, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Methoxypropylamine | HCID 1672 | — |
| Reactant | HCID 178526789 | HCID 178526789 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 178495257 | HCID 178495257 | 33.6% |
Reaction Steps
1.20 g (4.35 mmol) 2-(2-Chloro-pyridin-4-yl)-6-nitro-3H-imidazo[4,5-b]pyridine in 12 ml dry N-methylpyrrolidone (NMP) and 1.18 g (13 mmol) 3-methoxypropylamine were heated to 200 C in a closed vessel in a microwave reactor for 30 min. The solvent was removed under vacuum and the residue dissolved in a mixture of 20 ml ethyl acetate and 30 ml 5% aqueous HCl. The HCl phase was separated and brought to alkaline pH by addition of conc. ammonia. The alkaline aqueous phase was extracted with dichloromethane, and the organic phases were combined and dried. Evaporation and chromatography of the residue on silica in ethyl acetate/methanol mixtures gave 480 mg of the title product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07618964B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-c6c8135073c048d5a6af5f7ebcc666df |
| Source note | uspto-grants-2009_11 |