Methanol → Methyl 2-iodo-5-nitrobenzoate

HRID 381290

Reaktionsgleichung

Reaktionsgleichung von HRID 381290
[I:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:19]O>>[I:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([O:6][CH3:19])=[O:5]

Komponenten

4

Versuchsvorschrift

In a 5 liter 3 necked flask, 2-iodo-5-nitro-benzoic acid (100 grams) was dissolved in methanol (3000 ml). The flask was fitted with a reflux condenser and 50 ml of concentrated sulfuric acid was added carefully with cooling. After the completion of the addition, the contents were refluxed for 3 days until completion of the reaction. The reaction was followed by TLC. After the completion of the reaction, the reaction mixture was concentrated to 1000 ml and allowed to cool. The product crystalized as a light yellow colored powder. The solid material was filtered and washed with water and methanol and air-dried. The yield was 90 grams.

Aufarbeitung

  1. customThe flask was fitted with a reflux condenser
  2. temperaturewith cooling
  3. additionAfter the completion of the addition
  4. temperaturethe contents were refluxed for 3 days until completion of the reaction
  5. customAfter the completion of the reaction
  6. concentrationthe reaction mixture was concentrated to 1000 ml
  7. temperatureto cool
  8. customThe product crystalized as a light yellow colored powder
  9. filtrationThe solid material was filtered
  10. washwashed with water and methanol
  11. customair-dried

Quellen und Nachweise

ORD-Eintrag
ord-5ff507e7e7ad407ca2023eeafe0ea16d
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06306871B1

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