反应详情

LiAIH4 (3.1 g, 0.083 mol) was suspended in dry tetrahydrofuran (100 ml) in argon atmosphere. Ethyl 2-(2-bromo-3-methylphenyl)acetate (8.5 g, 0.033 mol) solved in dry tetrahydrofuran (50 ml) was added and the mixture was stirred at room temperature for 4 h. The mixture was cooled on ice and 3.1 ml of water was added dropwise, followed by 3.1 ml of 15% sodium hydroxide and then 9.3 ml of water. After 15 h. the solids were removed by filtration and washed thoroughly with tetrahydrofuran. The filtrate was removed under reduced pressure. Purification of the residue by filtrating through silica gel using methylene chloride:methanol (9:1) as eluent gave 7.0 g (98.6%) of the title compound as an oil.

1. additionwas added
2. additionwas added dropwise
3. customAfter 15 h. the solids were removed by filtration
4. washwashed thoroughly with tetrahydrofuran
5. customThe filtrate was removed under reduced pressure
6. customPurification of the residue
7. filtrationby filtrating through silica gel