Reaktion #49525

ord-fefce322f23643309993e528cf8bb506

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe precipitated solid was collected by filtration
  2. 2
    Waschenwashed with water
  3. 3
    Sonstigeby drying under reduced pressure
  4. 4
    SonstigeThe obtained solid was purified by slurry

Vorschrift

In a similar manner to Step 1 of Example 137, 3-chloro-4-methylbenzoic acid (1.00 g, 5.86 mmol) was dissolved in DMF (20 mL), and the solution was treated with EDCI (2.25 g, 11.7 mmol), HOBT monohydrate (792 mg, 5.86 mmol) and cumylamine (1.69 mL, 11.7 mmol). The reaction mixture was added with water. The precipitated solid was collected by filtration and washed with water, followed by drying under reduced pressure. The obtained solid was purified by slurry using diisopropylether to obtain 3-chloro-4-methyl-N-(1-methyl-1-phenylethyl)benzamide (1.64 g, yield 97%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745641B2uspto-grants-2010_06