Reaktion #417802

ord-23abeee68cbb4aab8b421e7f2967246d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe solvent and alkylating agent were removed in vacuo
  2. 2
    Sonstigeto afford a thick orange oil
  3. 3
    SonstigeCrystallization from ethanol-ether
  4. 4
    Sonstigeproduced 36 mg (90% yield)

Vorschrift

To 29 mg (0.06 mmol) of VII in 5 ml of chloroform was added 1 ml of methyliodide. After the mixture was stirred for 24 hours at room temperature, the solvent and alkylating agent were removed in vacuo to afford a thick orange oil. Crystallization from ethanol-ether produced 36 mg (90% yield), of a finely divided yellow powder: mp 135° C. decomposes; Rf(E)=0.06. Analysis calculated for C24H27N4O4I: C, 51.26; H, 4.84; N, 9.96. Found: C, 50.05; H, 5.23; N, 9.85. Fast atom bombardment mass spectrum: calculated for MW (435)+I-. Found: 435 (M+).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04897444uspto-grants-1990_01