HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethylamine → HCID 13136240, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | N,N-Dimethylpropargylamine | HCID 81643 | — |
| Reactant | HCID 13037329 | HCID 13037329 | — |
| Catalyst | Palladium(2+);tris(2-methylphenyl)phosphane;dichloride | HCID 9875586 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 13136240 | HCID 13136240 | 48.7% |
Reaction Steps
347 mg of 6-bromo-4-ethyl-beta-carboline-3-carboxylic-acid-ethylester, 32 mg of palladium-bis-(tri-o-tolylphosphine)-dichloride, 32 mg of cuprous iodide, 5 ml of diethylamine, 5 ml of N-methyl-2-pyrrolidone and 250 mg of 3-dimethylamino-1-propine are heated anhydrously and under nitrogen for 7.5 h at 80°-90° C. After concentration in an oil pump vacuum, the residue is chromatographed on 30 g of silica gel with methylene-chloride/methanol (10/2) as the eluant. The correspondingly consolidated fractions are separated by preparative film chromatography and 170 mg of 6-(3-dimethylamino-1-propinyl)-4-ethyl-beta-carboline-3-carboxylic-acid-ethylester is obtained in the form of an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04435403 |
| Source dataset | uspto-grants-1984_03 |
| ORD ID | ord-eedc684e5883449a8bf9875fd9980162 |
| Source note | uspto-grants-1984_03 |