HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 11387657, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 3,4,5-Trimethoxybenzoic Acid | HCID 8357 | — |
| Reactant | HCID 58911294 | HCID 58911294 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11387657 | HCID 11387657 | — |
Reaction Steps
To a solution of 1-(3-aminomethyl-pyrrolidin-1-yl)-6,6-bis-(4-fluoro-phenyl)-hexan-1-one (0.69 g, 1.78 mmol) in dry CH2Cl2 (40 ml) was added 3,4,5-trimethoxy benzoic acid (0.38 g, 1.78 mmol) under nitrogen. To the reaction was added EDC (0.68 g, 3.56 mmol) and DMAP (cat) and the reaction mixture stirred under nitrogen at room temperature overnight. The reaction was then concentrated under reduced pressure. The residue dissolved in ethyl acetate: water (10:1) (150 ml). The organic was washed with water (30 ml, 2×) and 10% NaOH (30 ml) and dried over MgSO4 and evaporated to dryness. The resulting residue was purified by column chromatography using CH2Cl2:CH3OH (15:1) to give a desired product in good yield
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07244758B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-7dcab0570dab43a3a3d1c834b6d28864 |
| Source note | uspto-grants-2007_07 |