Trichloroacetyl chloride → 2-Trichloroacetylmethylene-3-ethyl-benzothiazoline

HRID 1089404

Reaktionsgleichung

Reaktionsgleichung von HRID 1089404
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[CH3:12][C:13]1[S:14][C:15]2[CH:23]=[CH:22][CH:21]=[CH:20][C:16]=2[N+:17]=1[CH2:18][CH3:19].C(N(CC)CC)C.[Cl:31][C:32]([Cl:37])([Cl:36])[C:33](Cl)=[O:34]>C1(C)C=CC=CC=1>[Cl:31][C:32]([Cl:37])([Cl:36])[C:33]([CH:12]=[C:13]1[N:17]([CH2:18][CH3:19])[C:16]2[CH:20]=[CH:21][CH:22]=[CH:23][C:15]=2[S:14]1)=[O:34]

Komponenten

5

Edukt 3

HCID 6420Trichloroacetyl chlorideHCID 8471TriethylamineHCID 84711Benzothiazolium, 3-ethyl-2-methyl-, 4-methylbenzenesulfonate (1:1)

Produkt 1

HCID 543960172-Trichloroacetylmethylene-3-ethyl-benzothiazoline

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

10 g (28.6 mmol) of 2-methyl-3-ethyl-benzothiazolium p-toluenesulfonate are suspended in 150 ml of toluene, 6.8 g (67.2 mmol) of triethylamine are added and, at 5°-10° C. 6 g (33 mmol) of trichloroacetyl chloride, dissolved in a minor amount of toluene, are added dropwise. After three hours at room temperature, the ammonium salts are filtered off with suction, and the reaction solution is washed with water, dried over sodium sulfate and concentrated in vacuo. The product is caused to crystallize from the diisopropyl ether.

Aufarbeitung

  1. additionare added dropwise
  2. filtrationthe ammonium salts are filtered off with suction
  3. washthe reaction solution is washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto crystallize from the diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-d6002d5007a34608ac0debe48ba35e09
Quelldatensatz
uspto-grants-1990_10
Patentnummer
US04966828

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