HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 67995664, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 67995969 | HCID 67995969 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67995664 | HCID 67995664 | — |
Reaction Steps
Methyl chloroformate (0.20 mL) is added dropwise to a solution of 7-{2-[(S)-1-(4-bromo-phenyl)-ethylamino]-ethyl}-1,4-dioxa-spiro[4.5]decan-7-ol (0.50 g), triethylamine (0.4 mL), and pyridine (0.2 mL) in dichloromethane (10 mL) chilled in an ice bath. The solution is warmed to room temperature and stirred at this temperature overnight. Water is then added and the resulting mixture is extracted with dichloromethane. The combined extracts are washed with water (3×), dried (MgSO4), and concentrated. The residue is purified by HPLC on reversed phase (methanol/water) to give the title compound. Yield: 0.30 g (50% of theory); Mass spectrum (ESI+): m/z=442/444 (Br) [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08765744B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-60a7602edb0d410ab64fd6ed31e655af |
| Source note | uspto-grants-2014_07 |