반응 #47716
ord-dafb811201a54f49addfd5e8ddc343a5
반응 방정식
반응 조건
후처리
- 1온도After heating at 50° C. for 30 min
- 2온도The resulting mixture was maintained at 50° C. for 1hour
- 3온도cooled to room temperature (25° C.)
- 4추출The resulting mixture was extracted with ethyl acetate (3×50 mL)
- 5세척washed with saturated aqueous NaHCO3
- 6추출The ethyl acetate extract
- 7건조was dried over anhydrous sodium sulfate
- 8여과filtered
- 9농축concentrated under reduced pressure
- 10기타to yield the crude product
- 11기타The crude product was recrystallized from 2-propanol
실험 절차
(E)-2,4,6-Trimethoxystyryl-4-methoxy-3-nitrobenzylsulfoxide (1.3 mmol) was dissolved in a 2 to 1mixture of acetone and water (50 mL). The resulting mixture was heated to 50° C. After heating at 50° C. for 30 min, sodium dithionite (26.3 mmol) was added to the heated reaction mixture (portionwise over 20 minutes). The resulting mixture was maintained at 50° C. for 1hour, then cooled to room temperature (25° C.). Water (50 mL) was added to the cooled mixture. The resulting mixture was extracted with ethyl acetate (3×50 mL). The ethyl acetate extracts were combined and washed with saturated aqueous NaHCO3. The ethyl acetate extract was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to yield the crude product. The crude product was recrystallized from 2-propanol to afford the desired (E)-2,4,6-trimethoxy styryl-3-amino-4-methoxybenzylsulfoxide, as listed in Table 6.