HRID729931

反应详情

EQUATION

反应方程式

HRID 729931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Benzyltriethylammonium permanganate (0.281 g; 1.5 eq.) is added, at 5° C. and portionwise, to a solution of N-(4-benzyloxyphenyl)-N′-(3-methylbutyl)thiourea (0.200 g) and 3-dimethylamino-2,2-dimethylpropylamine (0.156 g; 2 eq.) in tetrahydrofuran (THF; 2.2 ml). The reaction medium is stirred for three days at room temperature. After filtration and concentration, the product is purified by chromatography on silica (eluent: methanol +0.1% acetic acid). The product, dissolved in dichloromethane, is washed with 1N sodium hydroxide. After drying and concentration, 0.067 g of N-(4-benzyloxyphenyl)-N′-(3-dimethylamino-2,2-dimethylpropyl)-N″-(3-methylbutyl)guanidine is obtained.

WORKUP

后处理

  1. filtrationAfter filtration and concentration
  2. customthe product is purified by chromatography on silica (eluent: methanol +0.1% acetic acid)
  3. dissolutionThe product, dissolved in dichloromethane
  4. washis washed with 1N sodium hydroxide
  5. customAfter drying
  6. concentrationconcentration