Methanol → HCID 20388954, Verbindung

HRID 426935Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 426935
[CH3:1][C:2]1[S:3][C:4]([CH2:7][CH2:8][C:9]([OH:11])=[O:10])=[CH:5][N:6]=1.S(=O)(=O)(O)O.[CH3:17]O>>[CH3:1][C:2]1[S:3][C:4]([CH2:7][CH2:8][C:9]([O:11][CH3:17])=[O:10])=[CH:5][N:6]=1

Komponenten

4

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 203889533-(2-methyl-1,3-thiazol-5-yl)propanoic acid

Produkt 1

HCID 20388954HCID 20388954, Verbindung

Versuchsvorschrift

A mixture of 31.7 g of the product of Step B, 3.2 ml of concentrated sulfuric acid and 300 ml of methanol was refluxed for 16 hours and was evaporated to dryness under reduced pressure. The residue was taken up in 100 ml of water and concentrated ammonium hydroxide was added thereto to adjust the pH to 12-13. The mixture was extracted with methylene chloride and the extracts were dried over magnesium sulfate and evaporated to dryness under reduced pressure to obtain 35 g of raw methyl 2-methyl-5-thiazole-propanoate. Reaction with hydrochloric acid resulted in the hydrochloride melting at 115° C.

Aufarbeitung

  1. temperaturewas refluxed for 16 hours
  2. customwas evaporated to dryness under reduced pressure
  3. additionconcentrated ammonium hydroxide was added
  4. extractionThe mixture was extracted with methylene chloride
  5. dry with materialthe extracts were dried over magnesium sulfate
  6. customevaporated to dryness under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-24817f9474c342b28b22206343f173d9
Quelldatensatz
uspto-grants-1979_10
Patentnummer
US04172137

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