(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 → 4-碘-3-甲基苯甲酸甲酯

HRID 840487

反应方程式

HRID 840487 反应方程式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:17]O>>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([O:7][CH3:17])=[O:6]

参与物

4

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HCID 1118四氧化硫HCID 15173221-(2-异丙基苯基)-2-硫脲

产物 1

HCID 2317574-碘-3-甲基苯甲酸甲酯

实验过程

24.4 g (0.093 mol) of 3-methyl-4-iodobenzoic acid and 250 ml of methanol were introduced into a round-bottomed flask and 2.5 ml of concentrated sulfuric acid were added dropwise. Heating was carried out at reflux for twelve hours, the reaction mixture was evaporated and the residue taken up in ethyl acetate and water. The organic phase was separated by settling, dried over magnesium sulfate and evaporated. The residue was triturated in methanol and filtered. 21.9 g (85%) of the expected methyl ester, with a melting point of 58°-59° C., were recovered.

后处理

  1. temperatureHeating
  2. temperatureat reflux for twelve hours
  3. customthe reaction mixture was evaporated
  4. customThe organic phase was separated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customThe residue was triturated in methanol
  8. filtrationfiltered
  9. custom21.9 g (85%) of the expected methyl ester, with a melting point of 58°-59° C., were recovered

来源与证据

ORD记录
ord-28e714b4d999404bbb4c92a95d3104a7
来源数据集
uspto-grants-2002_04
专利号
US06368608B1

关联笔记

加载中…