Methanol → Butanedioic acid, 2-methyl-, 1,4-dimethyl ester

HRID 53362

반응식

HRID 53362 반응식
[CH3:1][OH:2].[C:3]([CH2:5][CH:6]([CH3:11])[C:7]([O:9][CH3:10])=[O:8])#N.[OH2:12]>CCOCC>[CH3:11][CH:6]([CH2:5][C:3]([O:2][CH3:1])=[O:12])[C:7]([O:9][CH3:10])=[O:8]

참가 물질

5

반응물 3

HCID 887Methanol2회HCID 962WaterHCID 3016095Methyl 3-cyano-2-methylpropionate

생성물 1

HCID 15350Butanedioic acid, 2-methyl-, 1,4-dimethyl ester

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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.

후처리

  1. additionwas intermittantly added dropwise to the content in the flask at 100° C. at atmospheric pressure under the
  2. customwas removed outside the reaction system together with methanol
  3. 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. temperaturereflux of methoanol over a period of 5 hours

출처 및 근거

ORD 기록
ord-03a7689d03c14c53aebdf96c720c73e8
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05618953

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