HRID1713104

反应详情

EQUATION

反应方程式

HRID 1713104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 2-[2-(4-cyclobutyl-piperazin-1-yl)-2-oxo-ethyl]-1,2,3,4-tetrahydro-isoquinoline-6-carboxylic acid ethyl ester (610 mg, 1.58 mmol) in a mixture of THF-MeOH-water (3:1:1, 5 ml) cooled to 0° C. is added lithium hydroxide (76 mg, 3.16 mmol, 2.0 eq.). The mixture is stirred at rt overnight. The organic solvent is evaporated, and the residue is acidified to pH=5 with hydrochloric acid (2.0 N, about 1.58 ml). The resulting aqueous solution is evaporated to dryness, and the residue is extracted with a DCM-EtOH mixture (9:1, 10 ml×4). The combined organic solution is dried over sodium sulfate, and concentrated to give the title compound. MS (+VE) m/z 356.2 (M++1).

WORKUP

后处理

  1. customThe organic solvent is evaporated
  2. customThe resulting aqueous solution is evaporated to dryness
  3. extractionthe residue is extracted with a DCM-EtOH mixture (9:1, 10 ml×4)
  4. dry with materialThe combined organic solution is dried over sodium sulfate
  5. concentrationconcentrated