Reaktion #653798

ord-d7b0670bf3d4493391d9d4d4c1c681b1

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturunder reflux overnight
  3. 3
    Temperaturcooled
  4. 4
    Sonstigeevaporated in vacuo
  5. 5
    workup.ADDITIONA mixture of the resultant residue and NaOH (170 mg) in aqueous MeOH (90%, 25 mL)
  6. 6
    EinengenThe reaction mixture was concentrated
  7. 7
    FiltrationThe solids were collected by filtration
  8. 8
    Sonstigedried

Vorschrift

A mixture of 9H-carbazole-3-carboxylic acid (300 mg, 1.42 mmol), K2CO3 (800 mg) and methyl iodide (1 mL) in 25 mL of acetone was heated under reflux overnight, then cooled and evaporated in vacuo. A mixture of the resultant residue and NaOH (170 mg) in aqueous MeOH (90%, 25 mL) was stirred at 50° C. for 30 minutes. The reaction mixture was concentrated and acidified with diluted HCl. The solids were collected by filtration and dried to give the title compound (280 mg, 87%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06175015B1uspto-grants-2001_01