HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 131723076, 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 20716555 | HCID 20716555 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131723076 | HCID 131723076 | — |
Reaction Steps
1-(N-t-Butoxycarbonyl-2(S)-aminobutyryl)-5-trifluoromethoxy-indoline-2(S)-carboxylic acid (0.432 g, 1 mmol) and 2,2,2-trifluoroethylamine hydrochloride (0.271 g, 2 mmol) were dissolved in dried dichloromethane (20 ml) under nitrogen at 0° C., and triethylamine (0.7 ml, 5 mmol) was added followed by bis(2-oxo-3-oxazolidinyl)phosphinic chloride (0.509 g, 2 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 8:2 dichloromethane: diethyl ether as eluent to provide an off-white solid as the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06335360B1 |
| Source dataset | uspto-grants-2002_01 |
| ORD ID | ord-5e4820c9f37e458fa2bc493fb8fa67a3 |
| Source note | uspto-grants-2002_01 |