Pyridine → 1,1,1-Trifluoropropan-2-yl carbonochloridate

Temperature

0 °C

To a mixture of 1,1,1-trifluoro-2-propanol (114.1 mg, 10 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 colorless oil which was used directly in the next step.

1. additionThe flask containing the above reaction mixture
2. customwas put into a refrigerator overnight
3. filtrationfiltered
4. concentrationThe filtrate was concentrated in vacuo in ice both to colorless oil which

ORD record

ord-3863166ae333446ea655f4b72feb6f7e

Source dataset

uspto-grants-2012_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08232404B2