反应 #91908

ord-728e7a341e764f538ab3f60ccd3d628b

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度at reflux overnight under N2
  2. 2
    过滤The reaction was filtered
  3. 3
    浓缩concentrated
  4. 4
    其他Purification by silica gel chromatography (PE:EtOAc=5:1)

实验过程

The suspension of 5-oxo-5,6,7,8-tetrahydronaphthalen-2-yl trifluoromethanesulfonate (1.8 g, 6.1 mmol), 3-methylbenzene-1-thiol (0.76 g, 6.1 mmol), Pd2(dba)3 (142 mg, 0.153 mmol), Xantphos (177 mg, 0.306 mmol) and DIEA (1.58 g, 12.2 mmol) in 1,4-dioxane (60 mL) was stirred at reflux overnight under N2. The reaction was filtered and concentrated. Purification by silica gel chromatography (PE:EtOAc=5:1) gave 1.8 g (100%) of the title compound as an orange oil. [M+H] Calc'd for C17H16OS, 269. Found, 269.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09447046B2uspto-grants-2016_09