HRID1177432

反应详情

EQUATION

反应方程式

HRID 1177432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-(4-(1,3-dioxan-2-yl)-2-fluorophenyl)-5-(4-phenylocta-1,7-dien-4-yl)thiazolo[5,4-b]pyridine (0.580 g, 1.16 mmol) in 22 mL DCM under argon was added tricyclohexylphosphine[1,3-bis(2,4,6-trimethylphenyl)-4,5-dihydroimidazol-2-ylidene][benzylidene]ruthenium(IV) dichloride (0.0492 g, 0.0579 mmol). The flask was fitted with a water-cooled reflux condenser and heated to reflux. The reaction was checked after 4 h and judged complete. Silica gel (4 g) was added and the reaction mixture was dried, purified by ISCO, gradient, 0-100% EA/hexanes, to give 2-(4-(1,3-dioxan-2-yl)-2-fluorophenyl)-5-(1-phenylcyclohex-3-enyl)thiazolo[5,4-b]pyridine as a foam/oil which solidified to an off-white solid. MS (ESI) m/z: Calculated: 472.2; Observed: 473.2 (M++1).

WORKUP

后处理

  1. temperaturecooled
  2. temperaturereflux condenser
  3. temperatureheated to reflux
  4. additionSilica gel (4 g) was added
  5. customthe reaction mixture was dried
  6. custompurified by ISCO, gradient, 0-100% EA/hexanes