Halogenated amide ester and internal electron donor with same
A technology of halogenated amide ester and halogen, which is applied in the field of halogenated amide ester to achieve the effect of high molecular weight distribution
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[0161] Example
[0162] 1. Synthesis of halogenated amide ester
[0163] Ethyl 2-cyano-2-isobutyl-4-methylvalerate and ethyl 2-cyano-2-isopropyl-3-methylbutanoate:
[0164]
[0165] A 500-ml round bottom flask was equipped with a magnetic stirrer and charged with ethyl 2-cyanoacetate (11.3 g, 0.1 mol) and anhydrous DMF (120 ml). A solution of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) (30.4g, 0.2mol, 1.0 equivalent) in dry DMF (40ml) was added dropwise to the stirring solution. After the addition was complete, the mixture was stirred for another hour. The flask was cooled in an ice water bath, and a solution of iodide (0.2 mol, 1.0 equivalent) in DMF (40 ml) was added dropwise. The mixture was warmed to room temperature and stirred for another 14 hours, until all starting material was converted to product (monitored by GC). The mixture was poured into ice water, and extracted with diethyl ether. The combined ether extracts were washed with water and brine, and dried over magnesium...
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