HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 45118641, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 16787068 | HCID 16787068 | — |
| Product | HCID 45118641 | HCID 45118641 | — |
Reaction Steps
To a solution of 1-[4-(2-amino-propyl)-piperazin-1-yl]-ethanone (149 mg, 0.4 mmol) and triethylamine (TEA, 118 μl, 0.8 mmol) was added Lawesson's reagent (162 mg, 0.4 mmol) at RT. The reaction mixture was heated at reflux for 3 h to provide 1-[4-(2-aminopropyl)-piperazin-1-yl]-ethanethione (intermediate IVa). The solvent was evaporated and the residue was partitioned between ethyl ether and HCl (1 N), the organic layer was discarded and the aqueous layer was basified by addition of a saturated solution of K2CO3. The aqueous solution was extracted with ethyl acetate four times. The organic layers were combined, dried over sodium sulfate and evaporated. The crude mixture was used for the next coupling reaction. M+=202.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07491821B2 |
| Source dataset | uspto-grants-2009_02 |
| ORD ID | ord-d7a65ba9e5dc4672991d60756f442ae9 |
| Source note | uspto-grants-2009_02 |