تفاعل #1955892
ord-2ac69597353d41bda0e0257589f3accc
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1تركيزThe reaction was concentrated in vacuo
- 2workup.ADDITIONdiluted with EtOAc (200 mL)
- 3غسيلwashed with deionized water (2×150 mL)
- 4تجفيفThe organic layer was dried over MgSO4
- 5تركيزconcentrated
- 6أخرىdried in vacuo
- 7أخرىThe crude product was purified by flash column chromatography (silica, 0-20% EtOAc in hexane)
الإجراء التجريبي
A mixture of 4-(methylthio)phenylacetic acid (5.10 g, 28.0 mmol) and H2SO4 (0.155 mL, 2.80 mmol) in EtOH (150 mL) in a 500 mL round bottom flask, were stirred at 100° C. for 26 hours. The reaction was concentrated in vacuo, diluted with EtOAc (200 mL), washed with deionized water (2×150 mL), and then with brine (100 mL). The organic layer was dried over MgSO4, concentrated, and dried in vacuo. The crude product was purified by flash column chromatography (silica, 0-20% EtOAc in hexane) to give the title compound (5.95 g). MS m/e=211 (M+H)+.