Water → HCID 178527067, compound

Participants

Reaction Conditions

Reaction Steps

A fixed amount of base and certain solvent (see the table below for the type of base and solvent) are added to a 100 ml three-necked bottle under the protection of nitrogen, 10 ml solvent (the same as the above solvent) with a fixed amount of tetraethyl methylenediphosphonate (see the table below for molar weight) dissolved therein is dropwise added on the condition that magnetic stirring is performed and cold water bath is maintained within a range from 10 to 15° C., gas is discharged, the addition can be finished about half an hour later, and stirring is continued for reaction for 20 minutes. Then, 10 ml solvent (the same as the above solvent), with 2.1 g C-14 aldehyde having a formula (3B) (prepared in the embodiment 7, 0.010 mol) dissolved therein, is dropwise added on the condition that cold water bath is maintained at a particular temperature, the addition can be finished about half an hour later, and stirring is continued while the temperature is maintained for reaction for 20 minutes. 10 ml water and 20 ml ether are added to the reaction mixture solution, which is followed by stirring for 10 minutes and layering, organic layer is rinsed by 20 ml sodium hydride aqueous solution with the concentration of 10%, dried by magnesium sulfate and filtered, the solvent is dried by evaporation under reduced pressure to obtain 3,7,11-trimethyl-1,3,6,10-tetraene-dodecyl diethyl phosphonate crude product, which is light brown liquid. Measurement for gas phase content and calculation for yield are carried out, and the results are shown in the table below.

Provenance & Evidence