HRID517754

反应详情

EQUATION

反应方程式

HRID 517754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (1-methylethyl)amine (0.077 mL, 0.900 mmol) and formaldehyde (35% aqueous) (0.067 mL, 0.9 mmol) in methanol (4 mL) was stirred at room temperature for 1.5 h before adding trimethylsilyl azide (0.155 mL, 1.170 mmol) and 4-(trifluoromethyl)phenyl isocyanide (200 mg, 1.170 mmol, Fluorochem, Old Glossop, UK). After stirring for 2 days the solution was concentrated in vacuo. The resulting residue was purified using MDAP. Fractions containing product were combined and concentrated in vacuo. The resulting solid was redissolved in MeOH and passed through a 5 g NH2 ion exchange column to give the title compound as a white solid (75 mg).

WORKUP

后处理

  1. concentrationwas concentrated in vacuo
  2. customThe resulting residue was purified
  3. additionFractions containing product
  4. concentrationconcentrated in vacuo
  5. dissolutionThe resulting solid was redissolved in MeOH