Lithium Chloride → Methyl 3-(2-bromophenyl)propanoate

Temperature

160 °C

Dimethyl 2-(2-bromobenzyl)malonate (54.25 g) was dissolved in a mixture of dimethylsulfoxide (220 ml) and water (3.24 ml), and lithium chloride (15.27 g) was added. The mixture was stirred at 160° C. of a bath temperature for 7.5 hours. After the reaction mixture was left standing for cooling, the solvent was removed by distillation under reduced pressure. The residual concentrate was poured into water, extracted with toluene. The organic layer obtained was washed twice with water and once with a saturated aqueous saline, dried over sodium sulfate, the solvent was removed by distillation under reduced pressure, and the residual concentrate was distilled under reduced pressure (96°-98° C./0.5 mmHg) to give the title compound (30.05 g).

1. additionwas added
2. waitAfter the reaction mixture was left
3. temperaturefor cooling
4. customthe solvent was removed by distillation under reduced pressure
5. concentrationThe residual concentrate
6. additionwas poured into water
7. extractionextracted with toluene
8. customThe organic layer obtained
9. washwas washed twice with water and once with a saturated aqueous saline
10. dry with materialdried over sodium sulfate
11. customthe solvent was removed by distillation under reduced pressure
12. concentrationthe residual concentrate
13. distillationwas distilled under reduced pressure (96°-98° C./0.5 mmHg)

ORD record

ord-1a8a120b80ac42d28f83f1bfff1d0b12

Source dataset

uspto-grants-1997_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05594081