反応 #2069933

ord-16b8ab106e5d4b21bac8b71bbb71805e

反応方程式

c1ccc2c(c1)Sc1ccccc1S2
Thianthrene
O=[N+]([O-])O
nitric acid
O=S1c2ccccc2Sc2ccccc21
thianthrene-S-oxide

試薬

なし

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the reaction
  2. 2
    その他the reaction solution obtained
  3. 3
    その他to precipitate a crystal
  4. 4
    ろ過The crystal was collected by filtration
  5. 5
    その他recrystallized from acetonitrile

実験手順

Thianthrene (20 g) was refluxed in 300 ml of acetic acid, and 36 ml of dilute nitric acid was gradually added dropwise thereto. After allowing the reaction to proceed for 5 hours, the reaction solution obtained was poured in 1.2 liter of water to precipitate a crystal. The crystal was collected by filtration and then recrystallized from acetonitrile to obtain 12 g of thianthrene-S-oxide. 1H-NMR (400 MHz, CDCl3): δ 7.42 (t, 2H), 7.56 (t, 2H), 7.63 (d, 2H), 7.93 (d, 2H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07541131B2uspto-grants-2009_06