HRID383993

反应详情

EQUATION

反应方程式

HRID 383993 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 471 mg (2.0 mmol) of 4,4-dimethyl-1-phenyl-3,4-dihydroisoquinoline in MeOH (6 ml) was cooled to 0° C. and 151 mg (4.0 mmol) of NaBH4 were added in portions. After stirring for 3 h at RT a saturated aqueous NH4Cl solution was added. Then most of the methanol was removed under vacuum and the residue was extracted with EE. The organic phase was washed with brine, dried over Na2SO4, filtered and concentrated to small volume under vacuum. 19 mg (0.08 mmol, 4%) of 4,4-dimethyl-1-phenyl-1,2,3,4-tetrahydroisoquinoline were obtained as the residue, which was reacted further with no additional purification.

WORKUP

后处理

  1. additionwas added
  2. customThen most of the methanol was removed under vacuum
  3. extractionthe residue was extracted with EE
  4. washThe organic phase was washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated to small volume under vacuum