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

Temperature

0 °C

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 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-677c0583004846a88022b923f85a8aea

Source dataset

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08003796B2