反应详情

To a mixture of (2-bromo-5-nitrophenyl)methanol (6.32 g) and THF (150 mL) there were added diisopropylethylamine (5.21 mL) and methanesulfonyl chloride (2.32 mL) dropwise in that order at −10° C. under a nitrogen atmosphere. The mixture was stirred overnight at room temperature, and then ethyl acetate (400 mL) and water (200 mL) were added. The mixture was sufficiently shaken, and then the organic layer was separated oft washed with water (200 mL) and saturated aqueous sodium chloride (200 mL) in that order, and dried over anhydrous magnesium sulfate. The mixture was filtered to obtain a filtrate and the solvent in the filtrate was distilled off under reduced pressure to obtain the target compound (7.35 g) as a brown solid, which was used without purification as starting material for the following reaction (1c).

1. stirringThe mixture was sufficiently shaken
2. customthe organic layer was separated
3. washoft washed with water (200 mL) and saturated aqueous sodium chloride (200 mL) in that order
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationThe mixture was filtered
6. customto obtain a filtrate
7. distillationthe solvent in the filtrate was distilled off under reduced pressure