Bromine → 5-Bromo-3-methylthiophene-2-carbaldehyde

温度

100 °C

A solution of 3-methyl-thiophene-2-carboxaldehyde (12.0 g) in chloroform (50 ml) was added drop-wise to bromine (5.1 ml) in chloroform over 30 minutes and then heated to 100° C. for 140 minutes. The reaction mixture was diluted with chloroform and washed with 10% aqueous sodium thiosulfate solution, saturated aqueous bicarbonate solution and water. The organic solution was dried over magnesium sulfate and concentrated. The product isolated after evaporation of the solvent was further purified by vacuum distillation (122° C., 4 mbar) to give the title compound as a green oil.

1. washwashed with 10% aqueous sodium thiosulfate solution, saturated aqueous bicarbonate solution and water
2. dry with materialThe organic solution was dried over magnesium sulfate
3. concentrationconcentrated
4. customThe product isolated
5. customafter evaporation of the solvent
6. distillationwas further purified by vacuum distillation (122° C., 4 mbar)

ORDレコード

ord-68d53e10beee4f048db9f744e8204245

出典データセット

uspto-grants-2006_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07091237B2