HuagongsheHuagongshe Chemistry Print Report · For research reference only
Allylamine → HCID 18324818, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Allylamine | HCID 7853 | — |
| Reactant | HCID 9925711 | HCID 9925711 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18324818 | HCID 18324818 | 83.8% |
Reaction Steps
A mixture of allylamine (20 mL) and the hydrobromide salt of Step B (8.6 g) was heated at 100° C. under nitrogen for 30 minutes. The reaction mixture was cooled and partitioned between dichoromethane and 1N sodium hydroxide. The aqueous layer was extracted with dichloromethane, and the combined organic layers were dried over sodium sulfate and concentrated in vacuo to give a yellow oil. The crude material was dissolved in dichloromethane and absorbed onto a column of Merck-60 flash silica gel. Elution with 1:1 ethyl acetate-hexane followed by 80:20 dichloromethane-methanol containing 0.2% ammonium hydroxide gave the title compound (5.0 g, 83.8%) as a yellow oil which was used as such in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06340687B1 |
| Source dataset | uspto-grants-2002_01 |
| ORD ID | ord-faf4fb7ec35f4e2ea285941b710f1b17 |
| Source note | uspto-grants-2002_01 |