Reaktion #2170125

ord-d4c1347a32e045c4896f5fd912e19f82

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe mixture was then filtered
  2. 2
    Sonstigethe filtrate was evaporated to dryness
  3. 3
    workup.DISSOLUTIONThe solid residue was dissolved in 60ml hot water
  4. 4
    workup.ADDITION40 gm of potassium hydroxide was then added
  5. 5
    SonstigeThe product thus precipitated
  6. 6
    Filtrationwas filtered
  7. 7
    Sonstigecrystallized from acetone, m.p. 183° C

Vorschrift

2,4-Diamino-6-methyl pyrimidine was prepared by a modified procedure of Gabriel and Coleman (Ber., volume 34, page 1253, 1901). A mixture of 2-amino-4-chloro-6-methyl pyrimidine (9.0 gm) and alcoholic ammonia (225 ml), were heated in a steel bomb at 180° C for 6 hours. The mixture was then filtered, and the filtrate was evaporated to dryness. The solid residue was dissolved in 60ml hot water. The solution was cooled to room temperature, and 40 gm of potassium hydroxide was then added. The product thus precipitated, was filtered, and crystallized from acetone, m.p. 183° C. Yield: 5.5gm. U.V. spectrum data corresponded to those reported by Curd and Rose (J.C.S., page 98, 1949).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04083841uspto-grants-1978_04