反応 #1869197

ord-5389309b1db84247bd8965dc569dee38

反応方程式

Nc1ccc2c(c1)OCCO2
2,3-dihydro-benzo[1,4]dioxin-6-ylamine
O=C1CCC(=O)N1Br
N-bromosuccinimide
Nc1cc2c(cc1Br)OCCO2
oil
収率 93.0%
Nc1cc2c(cc1Br)OCCO2
7-Bromo-2,3-dihydro-benzo[1,4]dioxin-6-ylamine
収率 93.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他then evaporated
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in ether
  3. 3
    洗浄washed with water
  4. 4
    乾燥brine, dried
  5. 5
    その他evaporated

実験手順

A solution of 2,3-dihydro-benzo[1,4]dioxin-6-ylamine (1 g, 6.6 mmol) in tetrahydrofuran (15 ml) was cooled to −78 deg C. then treated with 1 drop of concentrated sulphuric acid followed by N-bromosuccinimide (1.2 g, 6.6 mmol). The mixture was allowed to warm to room temperature over 1 hour then evaporated. The residue was dissolved in ether, washed with water then brine, dried and evaporated to afford an oil (1.4 g, 93%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07498326B2uspto-grants-2009_03