Hydrochloric Acid → HCID 178425922, Verbindung

HRID 260346

Reaktionsgleichung

Reaktionsgleichung von HRID 260346
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[OH:10].C(N(CC)CC)C.Cl[S:19]([C:22]1[N:26]=[CH:25][NH:24][N:23]=1)(=[O:21])=[O:20].Cl>ClCCl>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[O:10][S:19]([C:22]1[N:26]=[CH:25][NH:24][N:23]=1)(=[O:21])=[O:20]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 106982,4,6-TrimethylphenolHCID 178527437HCID 178527437, Verbindung

Produkt 1

HCID 178425922HCID 178425922, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

4.1 g of 2,4,6-trimethylphenol was dissolved in 15 ml of dichloromethane, and 4.2 ml of triethylamine was added while stirring the solution. Further, 4.6 g of 3-chlorosulfonyl-1,2,4-triazole was gradually added while being cooled with ice and stirred. Then, the solution was stirred at room temperature for 14 hours. After that, 2N hydrochloric acid was added to separate the components. The organic layer was washed with water, and then it was dried with magnesium sulfate. Then, the solvent was removed by distillation, so that coarse crystals were obtained. The coarse crystals were recrystallized from n-hexane/ethyl acetate, so that 3.0 g of the titled compound was obtained.

Aufarbeitung

  1. temperaturewhile being cooled with ice
  2. stirringstirred
  3. stirringThen, the solution was stirred at room temperature for 14 hours
  4. customto separate the components
  5. washThe organic layer was washed with water
  6. dry with materialit was dried with magnesium sulfate
  7. customThen, the solvent was removed by distillation
  8. customso that coarse crystals were obtained
  9. customThe coarse crystals were recrystallized from n-hexane/ethyl acetate, so that 3.0 g of the titled compound
  10. customwas obtained

Quellen und Nachweise

ORD-Eintrag
ord-7b69206384364620b56e56db4f4fec5d
Quelldatensatz
uspto-grants-1996_06
Patentnummer
US05527818

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