HRID1466117

反应详情

EQUATION

反应方程式

HRID 1466117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 6-Oxo-5,6,7,8-tetrahydronaphthalene-2-carbonitrile (24 mg, 0.14 mmol) and 1-[2-(4-nitrophenyl)ethyl]piperazin-2-one (20 mg, 0.070 mmol) was treated with titanium(IV) isopropoxide (0.10 ml, 0.35 mmol) for 30 minutes. Then the reaction was diluted with ethanol (5 mL), and sodium cyanoborohydride (44 mg, 0.70 mmol) was added. The reaction was stirred at RT overnight. The reaction was diluted with EtOAc, washed with brine, dried over sodium sulfate, and concentrated to give the crude residue. The desired product was purified by reverse phase HPLC (AcCN-Water with 0.1% TFA). LC-MS (IE, m/z): 405 [M+1]+.

WORKUP

后处理

  1. additionwas added
  2. washwashed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated