(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 → 甲基丁二酸二甲酯

HRID 53362

反应方程式

HRID 53362 反应方程式
[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]

参与物

5

反应物 3

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮2 次HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 3016095Methyl 3-cyano-2-methylpropionate

产物 1

HCID 15350甲基丁二酸二甲酯

试剂、催化剂与溶剂 1

HCID 3283乙醚溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-03a7689d03c14c53aebdf96c720c73e8
来源数据集
uspto-grants-1997_04
专利号
US05618953

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