Acetic Anhydride → 5-Formamido-1-(2-hydroxyethyl)pyrazole

HRID 248334

Reaktionsgleichung

Reaktionsgleichung von HRID 248334
[C:1](OC(=O)C)(=[O:3])C.[OH:8][CH2:9][CH2:10][N:11]1[C:15]([NH2:16])=[CH:14][CH:13]=[N:12]1.C(=O)([O-])[O-].[K+].[K+]>C(O)=O>[OH:8][CH2:9][CH2:10][N:11]1[C:15]([NH:16][CH:1]=[O:3])=[CH:14][CH:13]=[N:12]1

Komponenten

5

Edukt 3

HCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 3202812-(5-amino-1H-pyrazol-1-yl)ethan-1-ol

Produkt 1

HCID 150777375-Formamido-1-(2-hydroxyethyl)pyrazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 284Formic AcidLösungsmittel

Versuchsvorschrift

A mixture of acetic anhydride (44.5 ml) and formic acid (22.3 ml) was stirred at ambient temperature for an hour. To this mixture was added 1-(2-hydroxyethyl)-5-aminopyrazole (30 g) at 0°-10° C., and the mixture was stirred under ice-cooling for 30 minutes. The mixture was poured into ice-cold water, adjusted to pH 10.5 with 40% aqueous potassium carbonate, and stirred under ice-cooling for 30 minutes. The mixture was extracted with a mixture of tetrahydrofuran and ethyl acetate 6 times. The organic layer was dried over magnesium sulfate and evaporated in vacuo to give 1-(2-hydroxyethyl)-5-formamidopyrazole (30.8 g).

Aufarbeitung

  1. stirringthe mixture was stirred under ice-
  2. temperaturecooling for 30 minutes
  3. additionThe mixture was poured into ice-cold water
  4. stirringstirred under ice-
  5. temperaturecooling for 30 minutes
  6. extractionThe mixture was extracted with a mixture of tetrahydrofuran and ethyl acetate 6 times
  7. dry with materialThe organic layer was dried over magnesium sulfate
  8. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-a11476a6a9584ddf9f0ba0f5a727b73f
Quelldatensatz
uspto-grants-1993_05
Patentnummer
US05210080

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