反应 #1387312
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05403953
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 4.9 mmol of lithium aluminum hydride are placed, under a nitrogen atmosphere, in 50 ml of ether. 3.3 mmol of 2-hydroxy-3-methylbenzoic acid, in solution in 40 ml of ether, are added dropwise while maintaining a reflux for 4 hours. The mixture is then cooled on ice and 12.5 ml of isopropanol and then 7.5 ml of a saturated sodium chloride solution are added. After 10 hours at room temperature, the mixture is filtered, rinsed with 1N hydrochloric acid and extracted with ether. The product is then obtained after silica column purification, using as eluent a pentane/ethyl acetate mixture (7/3). while maintaining a reflux for 4 hours the mixture is filtered rinsed with 1N hydrochloric acid extracted with ether The product is then obtained after silica column purification
来源 ID: ord-84cd4f891e4e4b168498664b6330168f