反応 #72743

ord-b8b50d6de82d48a99b4512bd5508fa78

溶媒

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他prepared
  2. 2
    温度It was cooled to room temperature
  3. 3
    ろ過filtered
  4. 4
    workup.ADDITIONThe filtrate was then poured into water
  5. 5
    ろ過It was then filtered
  6. 6
    その他to afford a solid
  7. 7
    洗浄the solid was washed with water
  8. 8
    その他dried in-vacuo

実験手順

A mixture of 6-bromo-2-methyl-4-nitro-1H-benzo[d]imidazole (prepared following the same procedure as Example 1) (3 g), 1-(bromomethyl)naphthalene (2.85 g) and K2CO3 (3.23 g) in DMF (100 mL) was stirred at 80° C. overnight. It was cooled to room temperature and filtered. The filtrate was then poured into water. It was then filtered to afford a solid and the solid was washed with water and then dried in-vacuo to afford the desired product (4.63 g, 100%). 1H NMR (300 MHz, DMSO-d6) δ ppm 2.54 (s, 3H), 6.16 (s, 2H), 6.32 (d, 1H, J=7.5 Hz), 7.33 (t, 1H, J=7.5 Hz), 7.61-7.72 (m, 2H), 7.87 (d, 1H, J=7.5 Hz), 8.01 (d, 1H, J=7.5 Hz), 8.14 (d, 1H, J=1.8 Hz), 8.19 (d, 1H, J=7.5 Hz), 8.28 (d, 1H, J=1.8 Hz); LC-MS: m/e=296 [M+1]+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541411B2uspto-grants-2013_09