반응 #2151003

반응 방정식

water

Potassium phthalimide

DMF

2-(iodomethyl)-2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran

→

title compound

수율 69.0%

2-[(2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran-2-yl)methyl]-1H-isoindole-1,3(2H)-dione

수율 69.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   기타synthesized in Reference Example 126
2. 2
   온도After that, the reaction solution was cooled to room temperature
3. 3
   기타to separate an organic layer
4. 4
   세척The organic layer was washed with water and saturated saline
5. 5
   기타dried
6. 6
   농축followed by concentration under reduced pressure
7. 7
   기타The residue was purified by silica gel chromatography (hexane-ethyl acetate 95:5-75:25)

실험 절차

Potassium phthalimide (702 mg, 3.79 mmol) was added to a solution of DMF (10 mL) containing 2-(iodomethyl)-2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran (1.00 g, 3.16 mmol) synthesized in Reference Example 126, and the mixture was stirred at 140° C. for 15 hours. After that, the reaction solution was cooled to room temperature, and water and ethyl acetate were added thereto to separate an organic layer. The organic layer was washed with water and saturated saline, and dried using anhydrous magnesium sulfate, followed by concentration under reduced pressure. The residue was purified by silica gel chromatography (hexane-ethyl acetate 95:5-75:25) to give 730 mg of the title compound (yield: 69%)

출처