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

温度

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 give a 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
5. customboth to give a colorless oil which

ORDレコード

ord-4cd0f1305fdd4b8ca6365b36aff1c416

出典データセット

uspto-grants-2011_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08076322B2