HRID403337

反应详情

EQUATION

反应方程式

HRID 403337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 1 L round-bottom flask was dissolved (E)-1-nitrohexa-1,5-diene (12.30 g, 97 mmol) and 2,3-difluorophenylboronic acid (38.2 g, 242 mmol) in dioxane (315 mL) to give a colorless suspension. Water (6.1 mL, 340 mmol) was added. The mixture was degassed with nitrogen and in a sonicator for 20 min. Sodium bicarbonate (4.06 g, 48.4 mmol) and (S)-(+2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (1.807 g, 2.90 mmol) and acetylacetonatobis(ethylene)rhodium (I) (0.749 g, 2.90 mmol) were added to the solution under nitrogen. The mixture was stirred at rt for 2 min, and then heated to 35° C. for 6 h under nitrogen. Reaction was continued for another 8 h at 35° C.

WORKUP

后处理

  1. customto give a colorless suspension
  2. customThe mixture was degassed with nitrogen and in a sonicator for 20 min
  3. temperatureheated to 35° C. for 6 h under nitrogen
  4. customReaction
  5. waitwas continued for another 8 h at 35° C.