تفاعل #1487563

ord-8a3bc6c8729f41fa8863915dca323293

ظروف التفاعل

درجة الحرارة
5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThe reaction mixture is extracted with EtOAc
  2. 2
    غسيلThe combined organic layers are washed with water
  3. 3
    تجفيفdried over sodium sulfate
  4. 4
    أخرىevaporated under vacuum
  5. 5
    أخرىThe crude product is purified by column chromatography over silica gel (100-200 mesh)

الإجراء التجريبي

2-(1,2,3,4-Tetrahydro-2-methylpyrido[4,3-b]indol-5-yl)-1-p-tolylethanol (1 equiv.) is refluxed with 25% sulfuric acid for 2 h. The reaction mixture is cooled to 5° C. with an ice-water bath. KOH (15% aq. solution) is added dropwise to the reaction mixture until pH 9-10 is achieved. The reaction mixture is extracted with EtOAc. The combined organic layers are washed with water followed by brine, dried over sodium sulfate and evaporated under vacuum. The crude product is purified by column chromatography over silica gel (100-200 mesh) using a gradient of MeOH-EtOAc (0-10%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08906925B2uspto-grants-2014_12