HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 53676026, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,2,2-Trifluoroethylamine hydrochloride | HCID 9772 | — |
| Reactant | Bis(2-oxo-3-oxazolidinyl)phosphinic chloride | HCID 152842 | — |
| Reactant | HCID 10915949 | HCID 10915949 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 53676026 | HCID 53676026 | — |
Reaction Steps
1-(N-t-Butoxycarbonyl-2(S)-aminobutyryl)-5-chloroindoline-2(S)-carboxylic acid (0.192 g, 0.5 mmol) and 2,2,2-trifluoroethylamine hydrochloride (0.205 g, 1.5 mmol) were dissolved in dried dichloromethane (5 ml) under nitrogen at 0° C., and triethylamine (0.63 ml, 4.5 mmol) was added followed by bis(2-oxo-3-oxazolidinyl)phosphinic chloride (0.382 g, 1.5 mmol). The temperature was allowed to rise to room temperature and the mixture was stirred at room temperature for 24 hours, then filtered. The filtrate was concentrated under vacuum to give a brown solid which was columned on silica gel using 7:3 petroleum spirit: ethyl acetate as eluent to provide a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06335360B1 |
| Source dataset | uspto-grants-2002_01 |
| ORD ID | ord-400c4bfbf1934e33b302c195a0fc5ecb |
| Source note | uspto-grants-2002_01 |