반응 #1182353

반응 방정식

5-bromo-2-hydroxy-benzaldehyde

K2CO3

toluene-4-sulfonic acid 3-ethyl-oxetan-3-ylmethyl ester

→

title compound

수율 47.8%

5-bromo-2-(3-ethyl-oxetan-3-ylmethoxy)-benzaldehyde

수율 47.8%

용매

DMF

반응 조건

후처리

1. 1
   온도cooled to room temperature
2. 2
   기타partitioned between water and ethyl acetate
3. 3
   세척The organic layer was washed with water for 3 times
4. 4
   건조dried over anhydrous Na2SO4
5. 5
   농축concentrated
6. 6
   기타The residue was purified by column chromatography

실험 절차

To a mixture of 5-bromo-2-hydroxy-benzaldehyde (14 g, 70 mmol), KI (5 g) and K2CO3 (19 g, 140 mmol) in DMF (100 mL) was added toluene-4-sulfonic acid 3-ethyl-oxetan-3-ylmethyl ester (19 g, 70 mmol). The mixture was heated at 140° C. for 2 h, and then cooled to room temperature, partitioned between water and ethyl acetate. The organic layer was washed with water for 3 times, dried over anhydrous Na2SO4 and concentrated. The residue was purified by column chromatography to give the title compound (10 g).

출처