HRID1253698

反应详情

EQUATION

反应方程式

HRID 1253698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Sodium t-Butylate (6.24 mmol, 3.0 eq.) was added to a stirred solution of tert-butyl 2,8-diazaspiro[4.5]decane-2-carboxylate (2.08 mmol, 1.0 eq.) and 4-bromo-2-(trifluoromethyl)pyridine (2.08 mmol, 1.0 eq.) in toluene (15 ml) and the reaction mixture was then degassed with N2. BINAP (0.12 mmol, 0.06 eq.) and Pd(OAc)2 (0.04 mmol, 0.02 eq.) were added and the reaction mixture obtained was heated at 120° C. for 12 h. The reaction mixture was filtered over Celite and the filtrate was concentrated in vacuo in order to obtain the crude product, which was purified by column chromatography (silica gel, 2% methanol in methylene chloride), in order to obtain the desired product. Yield: 62%

WORKUP

后处理

  1. customthe reaction mixture was then degassed with N2
  2. customthe reaction mixture obtained
  3. filtrationThe reaction mixture was filtered over Celite
  4. concentrationthe filtrate was concentrated in vacuo in order
  5. customto obtain the crude product, which
  6. customwas purified by column chromatography (silica gel, 2% methanol in methylene chloride), in order