反应详情

70 g (0.7 mol) of succinic anhydride and 96.6 g (0.7 mol) of veratrol were dissolved in 2000 ml of methylene chloride, and 237 g (1.75 mol) of anhydrous aluminum chloride was added thereto at room temperature. The mixture was stirred at the same temperature for 6 hours. The reaction solution was allowed to stand for 15 hours, and then 1600 ml of 6N hydrochloric acid was dropwise added under stirring. The mixture was stirred for 1 hour, and the organic layer was separated. 300 ml of water was added to the organic layer and adjusted to pH7.5 with a saturated sodium hydrogencarbonate aqueous solution. The water layer was separated, adjusted to pH2.5 with 6N hydrochloric acid and allowed to stand in a refrigerator for 2 days. The precipitated crystals were collected by filtration, washed and dried to obtain 106.8 g (yield: 64%) of 3-(3,4-dimethoxybenzoyl)propionic acid.

1. customat room temperature
2. waitto stand for 15 hours
3. stirringunder stirring
4. stirringThe mixture was stirred for 1 hour
5. customthe organic layer was separated
6. addition300 ml of water was added to the organic layer and adjusted to pH7.5 with a saturated sodium hydrogencarbonate aqueous solution
7. customThe water layer was separated
8. waitto stand in a refrigerator for 2 days
9. filtrationThe precipitated crystals were collected by filtration
10. washwashed
11. customdried