Bromine → 2-Bromo-6-hydroxybenzaldehyde

To a solution of 2-hydroxy-6-trimethylsilylbenzaldehyde (8.1 g) in carbon tetrachloride (160 ml) was added bromine (2.15 ml) dropwise at 0° C., and the mixture was stirred at room temperature overnight. To the mixture was added aqueous sodium hydrogencarbonate solution, and the layers were separated. The aqueous layer was extracted with dichloromethane and the organic layers were combined, washed with sodium thiosulfate solution, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel eluting with a mixture of hexane and toluene (4:1) to afford 6-bromo-2-hydroxybenzaldehyde (4.74 g).

1. customthe layers were separated
2. extractionThe aqueous layer was extracted with dichloromethane
3. washwashed with sodium thiosulfate solution
4. dry with materialdried over magnesium sulfate
5. customevaporated in vacuo
6. customThe residue was purified by column chromatography on silica gel eluting with a mixture of hexane and toluene (4:1)

ORDレコード

ord-e21d729b35684a0f84da65f981f76633

出典データセット

uspto-grants-1999_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05968985