反应详情

温度

0 °C

LiAlH4 (235 mg, 6.2 mmoles) was suspended in dry THF (10 mL) under nitrogen atmosphere. The suspension was cooled to 0° C. and 4-sulphamoyl-benzoic acid (500 mg, 2.48 mmoles, as a suspension in 10 mL of dry THF) was added. The resulting mixture was then refluxed for 18 hours. The reaction was quenched by addition of 3N HCl at 0° C. The quenched mixture was extracted with AcOEt, the organic layer was dried over Na2SO4 and evaporated to dryness. The crude material was purified by flash chromatography (SiO2, petroleum ether/AcOEt from 9/1 to 1/1) to yield the title compound in amount of 105 mg.

1. temperatureThe resulting mixture was then refluxed for 18 hours
2. customThe reaction was quenched by addition of 3N HCl at 0° C
3. extractionThe quenched mixture was extracted with AcOEt
4. dry with materialthe organic layer was dried over Na2SO4
5. customevaporated to dryness
6. customThe crude material was purified by flash chromatography (SiO2, petroleum ether/AcOEt from 9/1 to 1/1)