Acetic Acid → 2H-Benzotriazole, 2-phenyl-

HRID 2236066Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2236066
C1(C2C=CC=CC=2N[N:10]=[N:11][NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)C=CC=CC=1.C(O)(=O)C.C(O)(=O)C.C(O)(=O)C.I[C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1.ClCCl>O>[C:36]1([N:11]2[N:10]=[C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]3=[N:12]2)[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 6344DichloromethaneHCID 12217721Iodo benzene diacetateHCID 178420498HCID 178420498, Verbindung

Produkt 1

HCID 1540962H-Benzotriazole, 2-phenyl-Ausbeute 34 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

2-phenylazoaniline (3.47 g, 17.6 mmol) prepared above was placed in a 100-mL 1-neck round bottomed flask. Acetic acid (20 mL) and iodobenzene diacetate (6.23 g, 19.4 mmol) were added, in that order, resulting in an exotherm. The reaction was allowed to proceed for 1 hour during which time the mixture cooled to room temperature. Dichloromethane and water were added to the reaction mixture. The organic layer was separated and dried over MgSO4. The solution was filtered and concentrated using a rotary evaporator. The residue was purified on a silica gel column using dichloromethane as eluent. The fractions containing the desired product were combined and solvent removed. The solid was dried in a vacuum oven for 2 h. Yield: 34%.

Aufarbeitung

  1. customresulting in an exotherm
  2. customThe organic layer was separated
  3. dry with materialdried over MgSO4
  4. filtrationThe solution was filtered
  5. concentrationconcentrated
  6. customa rotary evaporator
  7. customThe residue was purified on a silica gel column
  8. additionThe fractions containing the desired product
  9. customsolvent removed
  10. customThe solid was dried in a vacuum oven for 2 h

Quellen und Nachweise

ORD-Eintrag
ord-a3dae15437e442f885108eed9e767164
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07714099B2

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