Acetic Acid → 2,3,4-Tribromo-5-(chloromethyl)thiophene

HRID 127758

Reaktionsgleichung

Reaktionsgleichung von HRID 127758
C=O.[ClH:3].[Br:4][C:5]1[C:9]([Br:10])=[C:8]([Br:11])[S:7][CH:6]=1.[C:12](O)(=O)C>>[Cl:3][CH2:12][C:6]1[S:7][C:8]([Br:11])=[C:9]([Br:10])[C:5]=1[Br:4]

Komponenten

5

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

4.07 G. (50 mmol) of formalin (37%) and 40 ml. of concentrated hydrochloric acid were added to a solution of 10.2 g. (33.3 mmol) of 3,4,5-tribromothiophene in 20 ml. of acetic acid. The resulting mixture was warmed to 70° C. After 6 hrs., 4.07 g. of formalin were added and heating was continued overnight. The resulting mixture was cooled, poured on ice water and extracted with ether. The organic phase was washed twice with water, sodium bicarbonate and water, dried and evaporated to give crude 2-chloromethyl-3,4,5-tribromothiophene.

Aufarbeitung

  1. temperatureheating
  2. waitwas continued overnight
  3. temperatureThe resulting mixture was cooled
  4. additionpoured on ice water
  5. extractionextracted with ether
  6. washThe organic phase was washed twice with water, sodium bicarbonate and water
  7. customdried
  8. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-9510259a80f744889a12dc20c83a48cf
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04256878

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