Reaktion #55500

ord-32cef9d776e644fa9ed2f82788d54e0e

Lösungsmittel

Reaktionsbedingungen

Temperatur
-15°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe organic phase is separated
  2. 2
    Waschenwashed with two 100 ml portions of water
  3. 3
    Trocknendried over sodium sulphate
  4. 4
    SonstigeThe solvent is evaporated

Vorschrift

A suspension of 369 g of cyanuric chloride in 1000 ml of ethyl acetate is cooled to -15° C. With good stirring, 124 g of isopropylamine are first added dropwise at -20° C. to -10° C. in the course of 21/2 hours, followed by 267 g of a 30% aqueous solution of sodium hydroxide in the course of one hour. The reaction mixture is stirred for a further 11/2 hours at the same temperature, then the organic phase is separated, washed with two 100 ml portions of water and dried over sodium sulphate. The solvent is evaporated, to yield an oil from which the 2,4-dichloro-6-isopropylamino-s-triazine precipitates in crystalline form after stirring with petroleum ether at low temperature. Melting point: 46°-47° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04220770uspto-grants-1980_09