تفاعل #43360

ord-08c55e9d266e442688fef7b33c0e6450

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةunder cooling with ice
  2. 2
    غسيلthen was washed with water and saturated brine
  3. 3
    تجفيفdried over anhydrous sodium sulfate
  4. 4
    تركيزConcentrating
  5. 5
    أخرىthe reaction liquid under reduced pressure
  6. 6
    أخرىthe residue was purified on silica gel column chromatography (KP—NH, ethyl acetate:hexane=1:20)

الإجراء التجريبي

Triethylamine (1.3 mL, 9.30 mmols) and acetyl chloride (0.6 mL, 8.46) were added to THF (20 mL) solution of (3S)-1-benzyl-3-hydroxypyrrolidine (1.5 g, 8.46 mmols) by the order stated, under cooling with ice, and stirred at the same temperature for an hour. Ethyl acetate was added to the reaction liquid which then was washed with water and saturated brine, and dried over anhydrous sodium sulfate. Concentrating the reaction liquid under reduced pressure, the residue was purified on silica gel column chromatography (KP—NH, ethyl acetate:hexane=1:20) to provide the title compound (1.68 g, 90%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07732456B2uspto-grants-2010_06