تفاعل #73748
ord-28d11bf4acba41d78da6c3b17b37123a
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةAfter cooling
- 2استخلاصextracted with ethyl acetate (150 mL)
- 3استخلاصThe organic extract
- 4غسيلwas washed with water (2×100 mL)
- 5تجفيفdried over sodium sulfate
- 6ترشيحfiltered
- 7أخرىThe solvent was removed in a rotary evaporator
- 8أخرىthe crude 33 thus obtained
- 9أخرىwas 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.