Acetone → HCID 21221128, Verbindung

HRID 1377174

Reaktionsgleichung

Reaktionsgleichung von HRID 1377174
[CH3:1][O:2][C:3]1[C:10]([O:11][CH3:12])=[C:9]([O:13][CH3:14])[CH:8]=[CH:7][C:4]=1[CH2:5]Cl.CC(C)=O.[I-:19].[Na+]>CCOCC>[CH3:1][O:2][C:3]1[C:10]([O:11][CH3:12])=[C:9]([O:13][CH3:14])[CH:8]=[CH:7][C:4]=1[CH2:5][I:19]

Komponenten

5

Edukt 3

HCID 180AcetoneHCID 5238Sodium IodideHCID 97491Toluene, alpha-chloro-2,3,4-trimethoxy-

Produkt 1

HCID 21221128HCID 21221128, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

46.64 g (215.2 mmol) of 2,3,4-trimethoxybenzyl chloride in 466 ml of abs. acetone are treated with 156.7 g (4.86 equivalents) of sodium iodide, and this mixture is stirred at RT for 2.75 h while excluding light. The reaction mixture is treated with approximately 3 l of (cold) ether, and the organic phase is washed once with 10 sodium thiophosphate solution and twice with saline (both kinds of solutions being cold). The combined aqueous phases are reextracted with ether. The combined organic phases are dried over Na2SO4 and evaporated on a RE at approximately 30° C. The residue, which is the desired title compound, is dried again under HV and subjected to further processing as a crude product. 1H-NMR (200 MHz, CDCl3): 7.03 and 6.59 (each d; each 1H); 4.47 (s, 2H); 4.05, 3.85 and 3.84 (each s, each 3H).

Aufarbeitung

  1. washthe organic phase is washed once with 10 sodium thiophosphate solution and twice with saline (both kinds of solutions
  2. dry with materialThe combined organic phases are dried over Na2SO4
  3. customevaporated on a RE at approximately 30° C
  4. customis dried again under HV

Quellen und Nachweise

ORD-Eintrag
ord-650d00b895b846988f0a51b96bfbbc18
Quelldatensatz
uspto-grants-1997_09
Patentnummer
US05663200

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