HRID1769131

反应详情

EQUATION

反应方程式

HRID 1769131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of the sulfonamide of Example 331 (c) (2.1 g, 4.54 mmol) in ethanol (125 mL) under nitrogen was added 10% Pd/C (0.6 g). The mixture was placed on a Parr hydrogenator at 50 psi of hydrogen for 2 hours, the catalyst was removed by filtration and the solvent was removed in vacuo. The residue was recrystallized from Et2O/MeOH, extracted with CH2Cl2, washed with water, then brine and was dried over MgSO4. The solvent was removed in vacuo to afford 1.41 g (82%) of N-methyl-N-(4-methoxybenzyl)-4-(2-(methoxycarbonyl)ethyl)phenylsulfonamide as a colorless oil.

WORKUP

后处理

  1. customthe catalyst was removed by filtration
  2. customthe solvent was removed in vacuo
  3. customThe residue was recrystallized from Et2O/MeOH
  4. extractionextracted with CH2Cl2
  5. washwashed with water
  6. dry with materialbrine and was dried over MgSO4
  7. customThe solvent was removed in vacuo