HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Butanol → HCID 13715336, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 12798005 | HCID 12798005 | — |
| Reactant | 4-[(2-Aminoethyl)amino]-4-oxobutan-2-yl nitrate | HCID 13715334 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 13715336 | HCID 13715336 | — |
Reaction Steps
4.2 g. 1-(3-cyanoindol-4-yloxy)-2,3-epoxypropane (see European patent specification No. 0,045,910) are suspended in 100 ml. n-butanol, mixed with 11.5 g. 2-(3-nitroxybutanoylamino)-ethylamine and stirred for 2 days at ambient temperature. After removal of the solvent, the residue is chromatographed on silica gel with methylene chloride/methanol (95:5 v/v) and methylene chloride/methanolic ammonia solution (95:5 v/v). From the appropriate fractions, after removal of the solvent, there are obtained 4.6 g. of base. By dissolving in methanol and adding the calculated amount of fumaric acid, there are obtained, after suction filtration, 3.9 g. (40% of theory) of the desired fumarate; m.p. 155°-156° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04863949 |
| Source dataset | uspto-grants-1989_09 |
| ORD ID | ord-a959de38b0a8486eaf8ef1a28814a2d3 |
| Source note | uspto-grants-1989_09 |