تفاعل #673003

ord-009c9b1af8864031848030af28aa7c35

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted with dichloromethane (3×40 mL)
  2. 2
    غسيلwashed with brine
  3. 3
    تجفيفdried with MgSO4
  4. 4
    أخرىthe solvent was removed in vacuo

الإجراء التجريبي

8-Bromo-4-methyl-7-trifluoromethyl-3,4,10,10a-tetrahydro-1H-pyrazino[1,2-a]indole-2-carboxylic acid tert-butyl ester (0.35 g, 0.8 mmol) were dissolved in dichloromethane (12 mL) and trifluoroacetic acid was added (3 mL). The mixture was stirred for 1 h, added to 1 N sodium hydroxide solution (50 mL) and extracted with dichloromethane (3×40 mL). Organic phases were pooled, washed with brine, dried with MgSO4 and the solvent was removed in vacuo. Chromatography on silica gel (dichloromethane/methanol 19:1) yielded the title compound as a colorless oil which was precipitated as HCl salt from diethylether (0.2 g; 73%). ISP-MS: m/e=335.2, 337.2 (M+H+), α D 20 = - 48.6 .

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06933387B2uspto-grants-2005_08