반응 #81640

반응 방정식

water

methanol

methyl 3-cyanoisobutyrate

methanol

→

dimethyl methylsuccinate

용매

ether

반응 조건

후처리

1. 1
   workup.ADDITIONwas intermittantly added dropwise to the content in the flask at 100° C. at atmospheric pressure under the
2. 2
   기타was removed outside the reaction system together with methanol
3. 3
   workup.ADDITIONand additional methanol in an amount of 2.6 times that of the methyl 3-cyanoisobutyrate was intermittantly added dropwise to the content in the flask at 100° C. at atmospheric pressure under the
4. 4
   온도reflux of methoanol over a period of 5 hours

실험 절차

The procedure in Example 1 was repeated to proceed with reaction except that in the second step of esterification, methanol in an amount by weight of 2.6 times that of the methyl 3-cyanoisobutyrate was intermittantly added dropwise to the content in the flask at 100° C. at atmospheric pressure under the reflux of methanol over a period of 5 hours; then at least 90% of water which was formed by the by-production of ether was removed outside the reaction system together with methanol; and additional methanol in an amount of 2.6 times that of the methyl 3-cyanoisobutyrate was intermittantly added dropwise to the content in the flask at 100° C. at atmospheric pressure under the reflux of methoanol over a period of 5 hours. As a result, dimethyl methylsuccinate was obtained at a yield of 97.6 mol % based on the fed methyl 3-cyanoisobutyrate, and by-production of dimethyl ether was at most 1 mol % based on the dimethyl methylsuccinate thus formed.

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