Reaktion #56116

ord-9689268751db44e2befdb5fba3d7f975

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThere were present in a stirrer
  2. 2
    Sonstigewere led in during one hour
  3. 3
    workup.STIRRINGstirred further for 4 hours
  4. 4
    Filtrationwas filtered off with suction
  5. 5
    SonstigeAfter the drying in the vacuum drying cabinet

Vorschrift

There were present in a stirrer apparatus protected against moisture 111 grams (1.0 mole) of pivaloyl cyanide, 150 grams (1.5 moles) of concentrated sulfuric acid and 150 ml of glacial acetic acid and there were led in during one hour under stirring at 0°-5° C.112 grams (2.0 moles) of isobutylene. Then the mixture was warmed up to room temperature and stirred further for 4 hours. Then the mixture was poured on 500 grams of ice and after thorough stirring the precipitated amide was filtered off with suction. After the drying in the vacuum drying cabinet, there were isolated 161 grams of analytically pure trimethyl pyruvic acid-N-t-butylamide which corresponds to a yield of 87% based on the acyl cyanide employed. The amide has a melting point of 65° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04224226uspto-grants-1980_09