反応式
[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]参加物
実験手順
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.
後処理
- additionwas intermittantly added dropwise to the content in the flask at 100° C. at atmospheric pressure under the
- customwas removed outside the reaction system together with methanol
- 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
- temperaturereflux of methoanol over a period of 5 hours
出典と根拠
- ORDレコード
- ord-03a7689d03c14c53aebdf96c720c73e8
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05618953
関連ノート
読み込み中…