HRID2417393

反应详情

EQUATION

反应方程式

HRID 2417393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-(4-Hydroxy-3-methoxy-phenyl)-5,6,6a,7,8,12b-hexahydro-benzo[k]phenanthridine-2-carbonitrile (0.1 mmol; 38.2 mg) was added at 10° C. to a mixture obtained by pre-treating sodium borohydride (600 mg) in 4 mL of THF with a mixture of THF (2 mL) and TFA (1.2 mL). The reaction mixture was reacted overnight before quenching with 1 mL of 10% HCl solution. The mixture was further heated for 1 hour before it was extracted using ammonium hydroxide and water. The organic phase was dried over magnesium sulfate and evaporated to dryness. The residue was purified using HPLC to yield compound 4-(2-Aminomethyl-5,6,6a,7,8,12b-hexahydro-benzo[k]phenanthridin-6-yl)-2-methoxy-phenol. Mass spectrum 369(M−17);in the presence of 0.1M ammonium acetate 385 (M−1) observed for negative ion mode.

WORKUP

后处理

  1. customobtained
  2. customThe reaction mixture was reacted overnight
  3. custombefore quenching with 1 mL of 10% HCl solution
  4. temperatureThe mixture was further heated for 1 hour before it
  5. extractionwas extracted
  6. dry with materialThe organic phase was dried over magnesium sulfate
  7. customevaporated to dryness
  8. customThe residue was purified