Nitric Acid → 4-Chloro-3,5-dimethyl-2-nitrophenol

HRID 641081

Reaktionsgleichung

Reaktionsgleichung von HRID 641081
[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([OH:9])=[CH:4][C:3]=1[CH3:10].[N+:11]([O-])([OH:13])=[O:12]>>[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([OH:9])=[C:4]([N+:11]([O-:13])=[O:12])[C:3]=1[CH3:10]

Komponenten

3

Edukt 2

HCID 944Nitric AcidHCID 27234-Chloro-3,5-dimethylphenol

Produkt 1

HCID 2318294-Chloro-3,5-dimethyl-2-nitrophenol

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

4-Chloro-3,5-dimethyl-phenol (20.0 g, 128 mmol) was dissolved in glacial acid (150 ml) and the solution was cooled to 5° C. Then nitric acid 65% (12.4 g, 128 mmol) was added dropwise while temperature was kept below 20° C. by external cooling. After the addition was complete stirring was continued for 1 hour at ambient temperature. The reaction mixture was poured into ice/water (1:1, 500 g) whereupon an orange solid precipitated. The solid was filtered off, washed with water and dried. Yield: 23.2 g (90.1%). 1H-NMR (DMSO-d6): δ=11.0 (s, 1H); 6.9 (s, 1H); 2.3 (s, 3H); 2.2 ppm (s, 3H).

Aufarbeitung

  1. customwas kept below 20° C. by external cooling
  2. additionAfter the addition
  3. customprecipitated
  4. filtrationThe solid was filtered off
  5. washwashed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-901e9f3418a44c99bb0da9a24cabec5d
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07695525B2

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