تفاعل #2161261

ord-e56fe79a6b7b4ec4b73f4b164cfe0b89

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe mixture was then concentrated
  2. 2
    workup.ADDITION25 mL of CH2Cl2 and 25 mL of water were added
  3. 3
    أخرىThe organic layer was separated
  4. 4
    استخلاصthe aqueous layer was extracted by additional amount of dichloromethane (2×10 mL)
  5. 5
    تجفيفdried over anhydrous Na2SO4
  6. 6
    تركيزconcentrated
  7. 7
    أخرىColumn chromatography on silica gel afforded 1.48 g (62%) of L as colorless solid

الإجراء التجريبي

To a stirred solution of 2.0 g (10.90 mmols) of 2,4,6-trichloropyrimidine in 25 mL of anhydrous ethanol at 0° C., was added drop wise a solution 0.79 g (10.90 mmols) of diethylamine in 5 mL of ethanol. This was followed by the addition of 2.3 mL (16.35 mmols) of triethylamine and the mixture was stirred for further 30 min. The mixture was then concentrated and 25 mL of CH2Cl2 and 25 mL of water were added. The organic layer was separated and the aqueous layer was extracted by additional amount of dichloromethane (2×10 mL) and the extracts were combined, dried over anhydrous Na2SO4 and concentrated. Column chromatography on silica gel afforded 1.48 g (62%) of L as colorless solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07919487B2uspto-grants-2011_04