تفاعل #45336
ord-9f39a994e7bf410e842925d20b4b4a44
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1استخلاصThe mixture was extracted with EtOAc (50 mL)
- 2غسيلthe organic extracts were washed with brine (25 mL)
- 3تجفيفdried over Na2SO4
- 4ترشيحfiltered
- 5تركيزconcentrated
- 6أخرىPurification by flash chromatography with 0% to 10% EtOAc/hexanes
الإجراء التجريبي
A solution of [3-iodo-5-(trifluoromethyl)phenyl]methanol (287 mg, 0.95 mmol) in CH2Cl2 (10 mL) was cooled to 0° C. and then Dess-Martin periodinane (604 mg, 1.42 mmol) was added. The reaction was slowly warmed to room temperature. After stirring at room temperature for twenty minutes, the reaction was poured into 1N NaOH (25 mL). The mixture was extracted with EtOAc (50 mL) and the organic extracts were washed with brine (25 mL), dried over Na2SO4, filtered, and concentrated. Purification by flash chromatography with 0% to 10% EtOAc/hexanes afforded 3-iodo-5-(trifluoromethyl)benzaldehyde. Rf=0.54 (15% EtOAc/hexanes). 1H NMR (CDCl3, 600 MHz) δ 9.98 (s, 1H), 8.39 (s, 1H), 8.19 (s, 1H), 8.09 (s, 1H).