Thionyl Chloride → 1-(Chloromethyl)-4,5-dimethoxy-2-nitrobenzene

HRID 1632788Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1632788
[N+:1]([C:4]1[CH:11]=[C:10]([O:12][CH3:13])[C:9]([O:14][CH3:15])=[CH:8][C:5]=1[CH2:6]O)([O-:3])=[O:2].S(Cl)([Cl:18])=O>>[N+:1]([C:4]1[CH:11]=[C:10]([O:12][CH3:13])[C:9]([O:14][CH3:15])=[CH:8][C:5]=1[CH2:6][Cl:18])([O-:3])=[O:2]

Komponenten

3

Edukt 2

HCID 24386Thionyl ChlorideHCID 660976-Nitroveratryl alcohol

Produkt 1

HCID 134492881-(Chloromethyl)-4,5-dimethoxy-2-nitrobenzeneAusbeute 86,4 %

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

570 g of 2-nitro-4,5-dimethoxybenzyl alcohol was added over 1 hour to 733 ml of thionyl chloride at 0° C. The solution was heated to 25° C. over 2 hours and to 50°-56° C. for 2 hours. The solution was cooled to 5° C. and the mixture was poured onto 12 l of ice water with stirring. The supernatant was poured off and the solid washed with water. The oily solid was blended with ice and water, filtered, and dried in a 40° C. vacuum oven to yield 535 g, 86.4% yield.

Aufarbeitung

  1. temperatureThe solution was cooled to 5° C.
  2. additionThe supernatant was poured off
  3. washthe solid washed with water
  4. filtrationfiltered
  5. customdried in a 40° C. vacuum oven
  6. customto yield 535 g, 86.4% yield

Quellen und Nachweise

ORD-Eintrag
ord-19529c06030648c9929e1791286fa877
Quelldatensatz
uspto-grants-1984_10
Patentnummer
US04477556

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