HRID339181

反应详情

EQUATION

反应方程式

HRID 339181 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

C-(6-Benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-methylamine (100 mg, 0.31 mmol) and 2-methylsulfanyl-4,5-dihydro-1H-imidazole hydroiodide (76 mg, 0.31 mmol) were added to 2 mL CH2Cl2, and the reaction mixture was heated to gentle reflux until all of the solvent was evaporated. The reaction mixture was heated to 150° C. for 30 minutes and then cooled. The crude mixture was basified by dropwise addition of aqueous NaOH solution, and then purified by preparative liquid chromatography (CH2Cl2/MeOH 90:10) on a short silica gel column. Removal of the solvent afforded 57 mg (47%) of (6-Benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-ylmethyl)-(4,5-dihydro-1H-imidazol-2-yl)-amine. MS: 370 (M+H)+.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto gentle reflux until all of the solvent
  3. customwas evaporated
  4. temperaturecooled
  5. additionThe crude mixture was basified by dropwise addition of aqueous NaOH solution
  6. custompurified by preparative liquid chromatography (CH2Cl2/MeOH 90:10) on a short silica gel column
  7. customRemoval of the solvent