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-e88afc2e6bc5457badbbc61a502e4dc0

Source dataset

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08513424B2