Phosphorus sulfide (P2S5) → Benzamide, thio-3,4,5-trimethoxy-

HRID 1421945Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1421945
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:14][CH3:15])[C:11]=1[O:12][CH3:13])[C:6]([NH2:8])=O.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:17]>C1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:14][CH3:15])[C:11]=1[O:12][CH3:13])[C:6]([NH2:8])=[S:17]

Komponenten

4

Edukt 2

HCID 14817Phosphorus sulfide (P2S5)HCID 183343,4,5-Trimethoxybenzamide

Produkt 1

HCID 3033195Benzamide, thio-3,4,5-trimethoxy-Ausbeute 122,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

500 mg of 3,4,5-trimethoxybenzamide was suspended in 15 ml of benzene. Thereto was added 526 mg of phosphorus pentasulfide. The mixture was refluxed for 30 minutes with heating. The solvent was removed by distillation. To the residue were added 5 ml of 10% sodium hydroxide and 5 ml of water. The mixture was stirred for 30 minutes. The reaction mixture was filtered, and the resulting solid was washed with small amounts of water and ethanol and dried to obtain 330 mg of 3,4,5-trimethoxythiobenzamide as a yellow powder.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 30 minutes
  2. temperaturewith heating
  3. customThe solvent was removed by distillation
  4. additionTo the residue were added 5 ml of 10% sodium hydroxide and 5 ml of water
  5. filtrationThe reaction mixture was filtered
  6. washthe resulting solid was washed with small amounts of water and ethanol
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-53dd710709b441e891cbfd7ed528bf34
Quelldatensatz
uspto-grants-2000_06
Patentnummer
US06080764

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