تفاعل #85825

ord-7694a110ba134784a421258096b9983e

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe mixture was stirred overnight at 60° C
  2. 2
    استخلاصextracted by EA
  3. 3
    غسيلthe organic layer was washed by brine
  4. 4
    تجفيفdried over Na2SO4
  5. 5
    تركيزconcentrated
  6. 6
    أخرىpurified by flash chromatography

الإجراء التجريبي

tetrahydro-2H-pyran-4-ol (850 mg, 8.32 mmol) was dissolved in DMF (10 mL), cooled to 0° C., NaH (500 mg, 10.4 mmol) was added and stirred for 45 minutes at room temperature, then 5-bromo-2-chloropyridine (2 g, 10.4 mmol) was added and the mixture was stirred overnight at 60° C. The mixture was poured into water, extracted by EA, the organic layer was washed by brine, dried over Na2SO4, concentrated and purified by flash chromatography, gave 1.7 g white solid. MS: (m/z): 258 (M−H)+, 260 (M+H)+

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434726B2uspto-grants-2016_09