HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → Ethyl 4-{[2-(thiophen-2-yl)ethyl]amino}benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Benzocaine | HCID 2337 | — |
| Reactant | Hexamethylphosphoramide | HCID 12679 | — |
| Reactant | 2-(2-Thienyl)ethyl methanesulphonate | HCID 3047723 | — |
| Solvent | Water | HCID 962 | — |
| Product | Ethyl 4-{[2-(thiophen-2-yl)ethyl]amino}benzoate | HCID 13079686 | — |
Reaction Steps
A mixture of 33.0 g. of ethyl p-aminobenzoate, 21.8 g. of 2-(2-thienyl)ethanol O-methanesulfonate (prepared as described in Example 49) and 100 ml. of hexamethylphosphoramide is heated in an oil bath at 125° C. for 16 hours. The mixture is chilled, diluted with 15 ml. of ethanol and 150 ml. of water. The mixture is extracted with ether and the ether extracts washed with water, dried over magnesium sulfate and concentrated in vacuo to give a crude oil. A sample of this oil is chromatographed over silica gel and the fractions containing the product are combined and recrystallized from hexane to give ethyl 4-[2-(2-thienyl)ethylamino]benzoate as yellow-tan crystals, m.p. 93°-95° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04185115 |
| Source dataset | uspto-grants-1980_01 |
| ORD ID | ord-e72014ae38674455b8b03b757c681c64 |
| Source note | uspto-grants-1980_01 |