HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 19600268, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Diethyl cyanophosphonate | HCID 76257 | — |
| Reactant | 4,5,6,7-Tetrahydrofuro[2,3-c]pyridine hydrochloride | HCID 19599907 | — |
| Reactant | HCID 22262276 | HCID 22262276 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19600268 | HCID 19600268 | — |
Reaction Steps
To a solution of 1.582 g (9.912 mmol) of 4,5,6,7-tetrahydrofuro[2,3-c]pyridine hydrochloride, 3.00 g (9.91 mmol) of 4-(2-phenyl-1,3-dithiolan-2-yl)benzoic acid and 5.53 ml (39.6 mmol) of triethylamine in 50 ml of N,N-dimethylformamide, 1.80 ml (11.9 mmol) of diethyl cyanophosphonate was added dropwise, followed by overnight stirring at room temperature. This mixture was poured into water and extracted with diethyl ether 3 times. The combined organic layer was dried over anhydrous sodium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=6/1 to 2/1) to yield the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05998433 |
| Source dataset | uspto-grants-1999_12 |
| ORD ID | ord-1353c563936b45f5a889466392ac03f2 |
| Source note | uspto-grants-1999_12 |