反应详情

A solution of lithium aluminium hydride (1M in THF, 18 ml, 18 mmol) was added to a solution of 2,4,6-trichlorobenzoyl chloride (4.35 g, 17.8 mmol ) in THF (70 ml) at 0°. After 1 h, water (685 μl), aqueous NaOH (3M, 685 μl) and water (2.06 ml) were added. The mixture was stirred vigorously for 1 h, the precipitate filtered off and the filtrate evaporated in vacuo to give a yellow solid. Recrystallisation from diisopropylether gave the title compound as white needles (2.63 g, 70%), m.p. 100-101°. δH (CDCl3) 7.35 (2 H, s, ArH), 4.91 (2 H, br s, CH2OH), 2.07 (1 H, br s, CH2OH).

1. filtrationthe precipitate filtered off
2. customthe filtrate evaporated in vacuo
3. customto give a yellow solid
4. customRecrystallisation from diisopropylether