反应详情

As illustrated by example 3, a dry solution of nitroform in a suitable inert organic solvent such as methylene chloride, 1,1-dichloroethane, 1,2-dichloroethane, 1,1,2-dichloroethane, etc., is added slowly to the iodomethyl 2-(trimethylsilyloxy)ethyl ether solution while the temperature of the solution is maintained in the range of from -50° C. to -80° C., and preferably from -70° C. to -80° C. Next, dry dimethylformamide is added to ionize the nitroform so that it will react with the iodomethyl ether. The solution is then allowed to warm slowly to a temperature of from about -5° C. to about +5° C. where it is kept until the reaction is completed. Pouring into ice water and then extraction into an organic solvent (e.g., methylene chloride) yields a crude 2,2,2-trinitroethyl 2-hydroxyethyl ether mixture.

1. temperatureis maintained in the range of from -50° C. to -80° C.
2. custompreferably from -70° C. to -80° C
3. temperatureto warm slowly to a temperature of from about -5° C. to about +5° C. where it
4. extractionextraction into an organic solvent (e.g., methylene chloride)