反应 #57547

ord-93ef0c03cac1401c888e831169151d18

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度This was refluxed for 5 h
  2. 2
    其他Reaction
  3. 3
    过滤filtered through a pad of Celite
  4. 4
    浓缩The organic was then concentrated in vacuo
  5. 5
    过滤The organic was then re-filtered through the same celite plug
  6. 6
    浓缩concentrated in vacuo

实验过程

3-Bromobenzenethiol (1 g, 5.3 mmol) was added to acetone (25 mL). Next was added potassium carbonate (1.46 g, 10.58 mmol) and 2-iodopropane (1.17 g, 6.88 mmol). This was refluxed for 5 h. Reaction was then cooled to rt and filtered through a pad of Celite. The organic was then concentrated in vacuo and taken up in ether at which time a white precipitate crashed out. The organic was then re-filtered through the same celite plug and concentrated in vacuo to provide 1.14 g (93.17%) of 1-bromo-3-isopropylsulfanyl-benzene as an oil. 1H-NMR (methylene chloride -d2) δ 7.54 (s, 1H), 7.37-7.31 (m, 2H), 7.18 (t, J=7.9 Hz, 1H), 3.50-3.36 (m, 1H), 1.31 (d, J=6.1 Hz, 6H); LC-MS RT: 4.15, [M+H]+: 233.2.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07420066B2uspto-grants-2008_09