Trichloroacetyl chloride → HCID 57098043, Verbindung

HRID 652986Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 652986
[CH2:1]([O:8][CH2:9][C:10]([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[CH2:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:31](Cl)(Cl)[C:32](Cl)=[O:33].P(Cl)(Cl)(Cl)=O>[Cu].[Zn].C(OCC)C>[CH2:1]([O:8][CH2:9][C:10]1([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])[CH2:31][C:32](=[O:33])[CH2:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

6

Edukt 3

HCID 6420Trichloroacetyl chlorideHCID 24813Phosphorus oxychlorideHCID 20196448HCID 20196448, Verbindung

Produkt 1

HCID 57098043HCID 57098043, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 10290809Zinc copper coupleKatalysatorHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A stirred mixture containing 7.18 g (18 mmol) of the compound prepared in (a) above, 75 ml of anhydrous diethyl ether and 1.4 g of zinc-copper couple was blanketed with nitrogen and treated dropwise at room temperature with a solution containing 3.63 g (20 mmol) of trichloroacetyl chloride and 3.06 g (20 mmol) of phosphorus oxychloride. After stirring the mixture at room temperature for 48 hours, the salts were filtered off and the filtrate concentrated in vacuo. The residue was then chromatographed on silica gel employing a mixture of petroleum ether and methyl-t-butyl ether in a ratio of 9:1 as the eluent to yield a yellow oil.

Aufarbeitung

  1. additiontreated dropwise at room temperature with a solution
  2. filtrationthe salts were filtered off
  3. concentrationthe filtrate concentrated in vacuo
  4. customThe residue was then chromatographed on silica gel employing
  5. additiona mixture of petroleum ether and methyl-t-butyl ether in a ratio of 9:1 as the eluent
  6. customto yield a yellow oil

Quellen und Nachweise

ORD-Eintrag
ord-fa953e530a6b4e9fa8d35264a3965288
Quelldatensatz
uspto-grants-1987_06
Patentnummer
US04673672

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