Dichlorofluoromethane → 1-Butyl-2-chloro-1-ethoxy-2-fluorocyclopropane

温度

20 °C

To a solution of 61.0 g. of 2-ethoxy-1-hexene, 135 ml. of 13.5 M potassium hydroxide and 217 g. of "18-crown -6" ether at -15° C. is added dropwise over 30 minutes at 0°, a 90 ml. portion of dichlorofluoromethane. After the addition, the mixture is placed in an ice bath. An exotherm raises the temperature to 20° C., whereupon the mixture is placed in a dry-ice/carbon tetrachloride bath to maintain the temperature at -5° C. to 0° C. After three hours at this temperature, the reaction mixture is diluted with water and extracted with ether. The ether extracts are combined, washed with water, then brine, dried over potassium carbonate and concentrated in vacuo to an oil. This oil is distilled through a 6 inch Vigreux column to provide 82 g. of the desired compound as a colorless liquid, b.p. 70°-71° C., 16 mm.

1. additionAfter the addition
2. customthe mixture is placed in an ice bath
3. customwhereupon the mixture is placed in a dry-ice/carbon tetrachloride bath
4. temperatureto maintain the temperature at -5° C. to 0° C
5. extractionextracted with ether
6. washwashed with water
7. dry with materialbrine, dried over potassium carbonate
8. concentrationconcentrated in vacuo to an oil
9. distillationThis oil is distilled through a 6 inch Vigreux column
10. customto provide 82 g

ORDレコード

ord-64a44d5f3cc143a290d2f0f98e68c855

出典データセット

uspto-grants-1981_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04297516