Nitric Acid → Thianthrene, 5-oxide

HRID 1982751ノート

反応式

HRID 1982751 の反応式
[CH:1]1[C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[N+]([O-])(O)=[O:16]>C(O)(=O)C.O>[CH:11]1[C:12]2[S:13][C:14]3[C:5](=[CH:4][CH:3]=[CH:2][CH:1]=3)[S:6](=[O:16])[C:7]=2[CH:8]=[CH:9][CH:10]=1

参加物

5

反応物 2

HCID 944Nitric AcidHCID 7109Thianthrene

生成物 1

HCID 73220Thianthrene, 5-oxide

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

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).

後処理

  1. customthe reaction
  2. customthe reaction solution obtained
  3. customto precipitate a crystal
  4. filtrationThe crystal was collected by filtration
  5. customrecrystallized from acetonitrile

出典と根拠

ORDレコード
ord-16b8ab106e5d4b21bac8b71bbb71805e
出典データセット
uspto-grants-2009_06
特許番号
US07541131B2

反応ノート

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