(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 → methyl 1H-benzimidazole-5-carboxylate hydrochloride

HRID 352842

反应方程式

HRID 352842 反应方程式
S(Cl)([Cl:3])=O.[N:5]1[C:9]2[CH:10]=[CH:11][C:12]([C:14]([OH:16])=[O:15])=[CH:13][C:8]=2[NH:7][CH:6]=1.[CH3:17]O>>[ClH:3].[N:5]1[C:9]2[CH:10]=[CH:11][C:12]([C:14]([O:16][CH3:17])=[O:15])=[CH:13][C:8]=2[NH:7][CH:6]=1

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 24386氯化亚砜HCID 4594561H-苯并咪唑-5-羧酸

产物 1

HCID 22710297methyl 1H-benzimidazole-5-carboxylate hydrochloride收率 97%

实验过程

Under ice cooling, thionyl chloride (2.30 ml) was added dropwise to methanol (50 ml). Then, 5-benzimidazolecarboxylic acid (5.00 g) was added, followed by heating under reflux for 5 hours. The reaction mixture was distilled under reduced pressure. The residue was pulverized in diethyl ether, followed by collection through filtration, whereby colorless crystals (6.36 g, 97%) was obtained.

后处理

  1. temperatureby heating
  2. temperatureunder reflux for 5 hours
  3. distillationThe reaction mixture was distilled under reduced pressure
  4. filtrationfollowed by collection through filtration

来源与证据

ORD记录
ord-f89a7e124718480098b5995cbd3b23e9
来源数据集
uspto-grants-2004_06
专利号
US06747023B1

关联笔记

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