تفاعل #466405
ord-eebc49c6774b4b758fa04e755bd90293
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.ADDITIONAfter the addition
- 2درجة الحرارةcooled to room temperature
- 3استخلاصextracted with Et2O (3×200 mL)
- 4غسيلThe combined organic extracts were washed with 10% aq. NaOH (100 mL) and brine (100 mL)
- 5تجفيفdried over MgSO4
- 6ترشيحfiltered
- 7تركيزconcentrated
الإجراء التجريبي
To a suspension of NaH (2.77 g, 115.6 mmol) in DMF (100 mL) at 0° C. was added a solution of 3-bromophenol 6-1 in DMF (40 mL) over 40 min. After the addition was complete, the solution was stirred for an additional 30 min. The solution was then treated with neat bromoacetaldehyde diethyl acetal (17.36 g, 115.6 mmol). The solution was heated at 100° C. for 8 h, cooled to room temperature, and extracted with Et2O (3×200 mL). The combined organic extracts were washed with 10% aq. NaOH (100 mL) and brine (100 mL), dried over MgSO4, filtered and concentrated to give 6-2 as a yellow oil.