Sodium Hydroxide → HCID 54002484, Verbindung

HRID 345505

Reaktionsgleichung

Reaktionsgleichung von HRID 345505
[CH3:1][O:2][C:3](=[O:15])[CH2:4][CH2:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=1.S(Cl)([Cl:19])(=O)=O.[OH-].[Na+]>C(Cl)Cl.CO>[CH3:1][O:2][C:3](=[O:15])[CH2:4][CH:5]([Cl:19])[C:6](=[O:14])[C:7]1[CH:8]=[CH:9][C:10]([CH3:13])=[CH:11][CH:12]=1

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 24648Sulfuryl chlorideHCID 288215Methyl 4-(4-methylphenyl)-4-oxobutanoate

Produkt 1

HCID 54002484HCID 54002484, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A stirred solution of 152.6 g (0.74 mole) of 3-(4-methylbenzoyl)propionic methyl ester in 225 mL of methylene chloride was cooled to -5° C. in methanol:ice bath. A solution of 109.9 g (66 mL, 0.81 mole) of sulfuryl chloride (97%) in 65 mL of methylene chloride was added dropwise at a rate which maintained the temperature at 0° C. The reaction mixture was allowed to warm to ambient temperature and stirred overnight. The reaction mixture was cooled to 0° C. in an ice bath and treated with 3N sodium hydroxide until just basic. The organic portion was separated, dried over magnesium sulfate and concentrated in vacuo (172.9 g). The oil was distilled at 125° C. (150 mm Hg) in 4 fractions. A sample of fraction 2 was sent for elemental analysis.

Aufarbeitung

  1. temperatureto warm to ambient temperature
  2. temperatureThe reaction mixture was cooled to 0° C. in an ice bath
  3. customThe organic portion was separated
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo (172.9 g)
  6. distillationThe oil was distilled at 125° C. (150 mm Hg) in 4 fractions

Quellen und Nachweise

ORD-Eintrag
ord-10f3278064f54a2e88bfce922bcbc51e
Quelldatensatz
uspto-grants-1991_10
Patentnummer
US05057534

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