تفاعل #219534

ord-1c58341a15d048099266fe6211fcbb02

الكواشف

لا شيء

ظروف التفاعل

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

المعالجة

  1. 1
    أخرىReaction
  2. 2
    درجة الحرارةwas warmed to room temperature
  3. 3
    غسيلMixture was washed successively with water (2×50 mL) and brine (30 mL)
  4. 4
    تجفيفOrganic layer was dried (magnesium sulfate)
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated in vacuo

الإجراء التجريبي

Triethlyamine (7.6 mL, 54 mmol), was added to a solution of 2-aminopyridine-3-carboxaldehyde (4.45 g, 36 mmol) in dichloromethane (70 mL). Mixture was cooled to 0° C. A solution of pivaloyl chloride (5.3 mL, 43 mmol) in dichloromethane (30 mL) was added to the mixture. Reaction was warmed to room temperature. Mixture stirred at room temperature for 63 hours. Mixture was washed successively with water (2×50 mL) and brine (30 mL). Organic layer was dried (magnesium sulfate), filtered and concentrated in vacuo. Silica gel chromatography afforded the title compound as off-white solid in 90% yield. (M+H)+=207.1.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07384931B2uspto-grants-2008_06