HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen chloride-ethyl acetate → HCID 22393754, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | HCID 22393654 | HCID 22393654 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22393754 | HCID 22393754 | 93.6% |
Reaction Steps
1.94 g (6.25 mmol) of tert-butyl 4-[3-(2-thienyl) propyl]-1-piperazinecarboxylate was dissolved in 20 ml of methanol, and 15 ml of a 4N hydrogen chloride-ethyl acetate solution was added. After completion of the reaction, the mixture was evaporated. The residue was adjusted to pH 11 with a 2N aqueous sodium hydroxide, then the objective product was extracted with chloroform and dried over anhydrous magnesium sulfate. The solvent was evaporated, to give 1.23 g (5.85 mmol, 93.6%) of the title compound as ayellow oil, as acrude product. 1H-NMR (400 MHz, CDCl3) δ 1.84-1.92 (m, 2H), 2.35-2.48 (m, 6H), 2.83-2.93 (m, 6H), 6.77-6.80 (m, 1H), 6.91 (dd, J 3.2 Hz, 5.2 Hz, 1H), 7.11 (dd, J=1.2 Hz, 5.2 Hz, 1H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06906072B1 |
| Source dataset | uspto-grants-2005_06 |
| ORD ID | ord-e4be5686d3a84ead89ed4e5841497381 |
| Source note | uspto-grants-2005_06 |