反应 #1810809

ord-9b19962bafd74275a9dbc508e2813d53

反应方程式

CN=C(SC)N(C)C1CCC(NC(=O)OCc2ccccc2)CC1
[4-(1,2,3-trimethyl-isothioureido)-cyclohexyl]carbamic acid benzylester
I
hydroiodide
[Cl-]
chloride
CCO
EtOH
NN.O
hydrazine monohydrate
CN=C(NN)N(C)C1CCC(NC(=O)OCc2ccccc2)CC1
[4-(3-Amino-1,2-dimethyl-guanidino)-cyclohexyl]-carbamic acid benzylester
Cl
hydrochloride

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A suspension obtained
  2. 2
    过滤is filtered
  3. 3
    其他the filtrate obtained
  4. 4
    其他The mixture obtained
  5. 5
    温度is refluxed for 2.5 hours and from the mixture
  6. 6
    其他obtained solvent
  7. 7
    其他is evaporated

实验过程

0.84 g of [4-(1,2,3-trimethyl-isothioureido)-cyclohexyl]carbamic acid benzylester in the form of a hydroiodide are stirred with 10 ml of of a strong basic ion exchanger in chloride form. A suspension obtained is filtered and the filtrate obtained is lyophilized. The lyophilisate is treated with 15 ml of EtOH and with 0.08 ml of hydrazine monohydrate. The mixture obtained is refluxed for 2.5 hours and from the mixture obtained solvent is evaporated. [4-(3-Amino-1,2-dimethyl-guanidino)-cyclohexyl]-carbamic acid benzylester in the form of a hydrochloride is obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07485632B2uspto-grants-2009_02