HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 1,1,1-Trifluoropropan-2-yl carbonochloridate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 1,1,1-Trifluoro-2-propanol | HCID 9774 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 1,1,1-Trifluoropropan-2-yl carbonochloridate | HCID 58270348 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a mixture of 1,1,1-trifluoro-2-propanol (114.1 mg, 1.0 mmol, Matrix Scientific) and triphosgene (98 mg, 0.33 mmol, Aldrich) in ethyl ether (10 mL) at −40° C. was added pyridine (80 μL, 1.0 mmol, EMD) in ethyl ether (1.0 mL) dropwise. The reaction mixture was warmed to 0° C. and stirred for 6 h. The flask containing the above reaction mixture was put into a refrigerator overnight and then filtered. The filtrate was concentrated in vacuo in ice both to give a colorless oil which was used directly in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08076322B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-4cd0f1305fdd4b8ca6365b36aff1c416 |
| Source note | uspto-grants-2011_12 |