m-Chloroperbenzoic acid → HCID 53978841, Verbindung

HRID 1073877Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1073877
[CH3:1][C:2]1([CH3:22])[CH2:7][CH:6]([C:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:4]=2[O:3]1.ClC1C=CC=C(C(OO)=[O:31])C=1>ClCCl>[CH3:1][C:2]1([CH3:22])[CH2:7][CH:6]([C:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][N+:9]=2[O-:31])[C:5]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:4]=2[O:3]1

Komponenten

4

Edukt 2

HCID 70297m-Chloroperbenzoic acidHCID 19895665HCID 19895665, Verbindung

Produkt 1

HCID 53978841HCID 53978841, VerbindungAusbeute 50,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

248 mg of 3,4-dihydro-2,2-dimethyl-4-(3-methyl-2-pyridyl)-6-nitro-2H-1-benzopyran were dissolved in 20 ml of dichloromethane at room temperature and 222 mg of m-chloroperbenzoic acid were added. After stirring at room temperature overnight the solution was washed in succession with sodium bisulphite solution, sodium bicarbonate solution and water. The organic phase was dried over sodium sulphate and evaporated. The resulting solid was triturated with diethyl ether, filtered off and recrystallized from acetonitrile to give 133 mg of 2-(3,4-dihydro-2,2-dimethyl-6-nitro-2H-1-benzopyran-4-yl) -3-methylpyridine N-oxide of melting point 218-220° C.

Aufarbeitung

  1. washwas washed in succession with sodium bisulphite solution, sodium bicarbonate solution and water
  2. dry with materialThe organic phase was dried over sodium sulphate
  3. customevaporated
  4. customThe resulting solid was triturated with diethyl ether
  5. filtrationfiltered off
  6. customrecrystallized from acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-8468e3676a0d408d8189c07d4a963190
Quelldatensatz
uspto-grants-1990_11
Patentnummer
US04971982

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