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Hydrochloric Acid → HCID 20285690, Verbindung

HRID 1764593
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1764593
[Cl:1][C:2]1[S:3][C:4]([Cl:8])=[CH:5][C:6]=1C.C=O.[ClH:11].CCO[CH2:15][CH3:16]>[Cl-].[Zn+2].[Cl-]>[Cl:11][CH2:6][C:5]1[C:15]([CH3:16])=[C:2]([Cl:1])[S:3][C:4]=1[Cl:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 3283Diethyl EtherHCID 2689102,5-Dichloro-3-methylthiophene

Produkt 1

HCID 20285690HCID 20285690, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3007855ZincchlorideKatalysator

Versuchsvorschrift

A mixture of 61.59 g. (0.368 mol) of 2,5-dichloro-3-methylthiophene, 13.1 g. of paraformaldehyde and 3.1 g. of zinc chloride was heated to 55° C. Hydrogen chloride gas was passed through the mixture for 7.25 hours. The resulting mixture was cooled and poured into a mixture of ether and ice water. The organic phase was separated and washed with sodium chloride solution, sodium bicarbonate solution and sodium chloride solution again. Evaporation of the dried solvent gave a dark brown oil which was distilled under reduced pressure to yield 3-chloromethyl-2,5-dichloro-4-methylthiophene as a pale yellow liquid, b.p. 87°-92° C./0.75 mm.

Aufarbeitung

  1. additionA mixture of 61.59 g
  2. temperatureThe resulting mixture was cooled
  3. customThe organic phase was separated
  4. washwashed with sodium chloride solution, sodium bicarbonate solution and sodium chloride solution again
  5. customEvaporation of the dried solvent
  6. customgave a dark brown oil which
  7. distillationwas distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-62907893e46a44dd9990e189157a856b
Quelldatensatz
uspto-grants-1978_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04116975

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