HRID1941481

反应详情

EQUATION

反应方程式

HRID 1941481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of dimethylsulphide (7 μl, 0.1 mmol), rhodium (II) acetate (2 mg, 0.005 mmol) and N-(4-methoxybenzylidene)toluene-p-sulphonamide (144 mg, 0.5 mmol) in dichloromethane (2 ml) was added phenyldiazomethane (prepared as in Example 36; 8.96 ml of a 0.067M solution in t-butylmethylether) over a period of 12 hours. Upon completion of the addition the solvent was removed in vacuo and the residue was chromatographed using silica gel eluting with 15:85 ethyl acetate:petrol to give the title compound (96 mg, 51%). δH (CDCl3) 7.62(2H), 6.75-7.45(11H,m), 4.35(1H,d,J=6 Hz), 4.18(1H,d,J=6 Hz), 3.62(3H,s), 2.35(3H,s)ppm.

WORKUP

后处理

  1. customprepared as in Example 36
  2. additionUpon completion of the addition the solvent
  3. customwas removed in vacuo
  4. customthe residue was chromatographed