HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 17973765, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethanamine, 2-fluoro-, hydrochloride | HCID 9995 | — |
| Reactant | HCID 17973764 | HCID 17973764 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 17973765 | HCID 17973765 | — |
Reaction Steps
A solution of 2-fluoroethylamine hydrochloride (1.08 g, 10.9 mmol; prepared as described in J. Med. Chem. 9 (1966), 892-911) in 30 mL of absolute MeOH was treated with triethylamine (2.50 mL, 1.76 g, 17.4 mmol) at 0° C. Solid 4-bromomethyl-3-(4-chlorophenyl)-2,2-dioxo-2-thia-1-aza-spiro[4.4]non-3-ene (1.64 g, 4.35 mmol; described during the preparation of Intermediate 6) was added. The resulting mixture was stirred for 16 h at ambient temperature and concentrated to dryness under reduced pressure. The residue was purified by column chromatography on silica gel using dichloromethane/methanol as eluent to yield the title intermediate. Yield: 1.00 g (64%); MS (IS): 359.1 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07396846B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-10b479b70c7e49499a473f347276165d |
| Source note | uspto-grants-2008_07 |