تفاعل #73748

ord-28d11bf4acba41d78da6c3b17b37123a

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling
  2. 2
    استخلاصextracted with ethyl acetate (150 mL)
  3. 3
    استخلاصThe organic extract
  4. 4
    غسيلwas washed with water (2×100 mL)
  5. 5
    تجفيفdried over sodium sulfate
  6. 6
    ترشيحfiltered
  7. 7
    أخرىThe solvent was removed in a rotary evaporator
  8. 8
    أخرىthe crude 33 thus obtained
  9. 9
    أخرىwas used in the next step without further purification

الإجراء التجريبي

A solution of 32 (1.5 g, 3.96 mmol) in anhydrous tetrahydrofuran (16 mL) was stirred under nitrogen at room temperature and 1M ortho-methoxyphenyl magnesium bromide in tetrahydrofuran (6 mL, 1.5 equiv.) was slowly added. Stirring was continued at room temperature for 30 min and at 60° C. for 3 hr. After cooling, the reaction mixture was poured on saturated ammonium chloride (100 mL) and extracted with ethyl acetate (150 mL). The organic extract was washed with water (2×100 mL), dried over sodium sulfate and filtered. The solvent was removed in a rotary evaporator and the crude 33 thus obtained was used in the next step without further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08541522B2uspto-grants-2013_09