HRID2383314

反应详情

EQUATION

反应方程式

HRID 2383314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1,1-dimethylethyl 1-[2-(butyloxy)-2-oxoethyl]-6-cyano-5-methyl-3,4-dihydro-2(1H)-isoquinolinecarboxylate (Preparation 18; 2.15 g, 5.56 mmol) in ethanol (10 ml) and diethyl ether (40 ml) was added lithium borohydride (2M solution in tetrahydrofuran, 4.17 ml; 8.34 mmol) at 25° C. under nitrogen. After 1.5 h at 25° C., the solvent was removed, and the residue dissolved in ethyl acetate. The solution was washed with 1N hydrochloric acid, and the aqueous layer further extracted with ethyl acetate. The combined organic phases were washed with saturated sodium bicarbonate, dried over MgSO4 and concentrated in vacuo to give the title compound (1.70 g) as a white foam.

WORKUP

后处理

  1. customthe solvent was removed
  2. dissolutionthe residue dissolved in ethyl acetate
  3. washThe solution was washed with 1N hydrochloric acid
  4. extractionthe aqueous layer further extracted with ethyl acetate
  5. washThe combined organic phases were washed with saturated sodium bicarbonate
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo