Nitric Acid → Thianthrene, 5-oxide

HRID 1982751

Reaktionsgleichung

Reaktionsgleichung von HRID 1982751
[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

Komponenten

5

Edukt 2

HCID 944Nitric AcidHCID 7109Thianthrene

Produkt 1

HCID 73220Thianthrene, 5-oxide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-16b8ab106e5d4b21bac8b71bbb71805e
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07541131B2

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