تفاعل #409258

معادلة التفاعل

NaH

3-bromophenol

bromoacetaldehyde diethyl acetal

→

3-2

1-Bromo-3-(2,2-diethoxy-ethoxy)-benzene

المذيبات

DMF

DMF

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONAfter the addition
2. 2
   درجة الحرارةcooled to room temperature
3. 3
   استخلاصextracted with Et2O (3×200 mL)
4. 4
   غسيلThe combined organic extracts were washed with 10% aq. NaOH (100 mL) and brine (100 mL)
5. 5
   تجفيفdried over MgSO4
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated

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 3-1 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 3-2 as a yellow oil.

المصدر