HRID1928484

反应详情

EQUATION

反应方程式

HRID 1928484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

To the above described N-tert-butyl-3-[6′-(tetrahydro-pyran-2-yloxymethyl)-4′-(4-trifluoromethyl-phenyl)-[2,2′]bipyridinyl-6-yl]-benzenesulfonamide (0.550 g, 0.88 mmol) was added TFA (5 mL) and the reaction mixture was stirred at 23° C. for 18 h. The mixture was poured into 3 N NaOH-solution (100 ml) and stirred at 23° C. for 15 min, then partitioned between EtOAc and water, the organic layer was washed with saturated NaHCO3 solution and dried over MgSO4. Removal of the solvent in vacuum left a crude product which was triturated with diethyl ether to give the title compound as an off-white solid (0.100 g, 23%). MS (ISP) 486.0 [(M+H)+]; mp 213° C. (dec.).

WORKUP

后处理

  1. stirringstirred at 23° C. for 15 min
  2. custompartitioned between EtOAc and water
  3. washthe organic layer was washed with saturated NaHCO3 solution
  4. dry with materialdried over MgSO4
  5. customRemoval of the solvent in vacuum
  6. waitleft a crude product which
  7. customwas triturated with diethyl ether