海萝胶 → 苯并咪唑-5-甲酸甲酯

HRID 1419122

反应方程式

HRID 1419122 反应方程式
[N:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]([OH:12])=[O:11])=[CH:9][C:4]=2[NH:3][CH:2]=1.[CH3:13]O.Cl>O1CCOCC1>[N:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]([O:12][CH3:13])=[O:11])=[CH:9][C:4]=2[NH:3][CH:2]=1

参与物

5

反应物 3

HCID 313海萝胶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 4594561H-苯并咪唑-5-羧酸

产物 1

HCID 2779733苯并咪唑-5-甲酸甲酯

试剂、催化剂与溶剂 1

HCID 312751,4-二氧六环溶剂

实验过程

A mixture of 10 g of 5-benzimidazolecarboxylic acid, 150 ml of methanol and 100 ml of a 4N solution of hydrogen chloride in 1,4-dioxane was agitated ultrasonically for 4 hours. At the end of this time, the solvent was removed by distillation under reduced pressure, after which 300 ml of methanol and 3.5 g of lithium borohydride were added to the residue and the mixture was stirred for 1 hour. The solvent was then removed by evaporation under reduced pressure and the residue was mixed with an aqueous solution of sodium chloride, after which it was extracted with ethyl acetate. The solvent was removed by distillation under reduced pressure, to give 5.44 g of the title compound, melting at 136°-138° C.

后处理

  1. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  2. additionafter which 300 ml of methanol and 3.5 g of lithium borohydride were added to the residue
  3. stirringthe mixture was stirred for 1 hour
  4. customThe solvent was then removed by evaporation under reduced pressure
  5. additionthe residue was mixed with an aqueous solution of sodium chloride
  6. extractionafter which it was extracted with ethyl acetate
  7. customThe solvent was removed by distillation under reduced pressure

来源与证据

ORD记录
ord-c11418e650954deeae25fbb9abf65142
来源数据集
uspto-grants-1999_03
专利号
US05886014

关联笔记

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