HRID991459

反应详情

EQUATION

反应方程式

HRID 991459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1-(4-oxo-1-phenyl-1,3,8-triazaspiro[4.5]dec-8-yl)cycloheptane-carbonitrile (323 mg, 0.916 mmol) in THF (6 ml) was added phenylmagnesium bromide (3M solution in diethyl ether, 3.05 ml, 9.16 mmol) at room temperature. Then the reaction mixture was stirred at room temperature for 24 h. The reaction mixture was poured into ice water, then extracted with CH2Cl2. The extracts combined were dried (Na2SO4), filtered, and concentrated. The residue was purified by preparative TLC (CH2Cl2/MeOH:10/1 to give 70.5 mg (19.1%) of title compound.

WORKUP

后处理

  1. extractionextracted with CH2Cl2
  2. dry with materialThe extracts combined were dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by preparative TLC (CH2Cl2/MeOH