تفاعل #1106676

معادلة التفاعل

Catechol

potassium carbonate

2-Chloromethyl-3-chloro-1-propene

→

3-methylene-3,4-dihydro-2H-benzo[b][1,4]dioxepine

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated
2. 2
   درجة الحرارةto reflux for one hour
3. 3
   درجة الحرارةat reflux for 24 hours
4. 4
   ترشيحfiltered
5. 5
   أخرىThe filtrate was evaporated
6. 6
   workup.ADDITIONthe residue was diluted with water
7. 7
   استخلاصextracted with diethyl ether (3×)
8. 8
   تجفيفThe combined organic solution was dried over MgSO4
9. 9
   تركيزconcentrated

الإجراء التجريبي

Catechol (5.09 g, 46.2 mmol) and potassium carbonate were combined in acetonitrile and heated to reflux for one hour. 2-Chloromethyl-3-chloro-1-propene (5.78 g, 46.2 mmol) was added and the reaction was continued at reflux for 24 hours. The solution was cooled to room temperature and filtered. The filtrate was evaporated and the residue was diluted with water and extracted with diethyl ether (3×). The combined organic solution was dried over MgSO4 and concentrated. Chromatography (2% ethyl ether in hexane) yielded 3-methylene-3,4-dihydro-2H-benzo[b][1,4]dioxepine as a colorless oil.

المصدر