Methacrylic Acid → 2-Methyl-3-(trichlorogermyl)propanoic acid

Temperature

5 °C

84.7 ml (0.1 mol) of methacrylic acid was added dropwise over 5 minutes to 18 g (0.1 mol) of crude trichlorogermane which had been cooled to 5° C. in an ice bath. The mixture was stirred at the same temperature for one hour and then at room temperature for 1.5 hour. The precipitated crystal was filtered by suction, washed with 10 ml of n-hexane which had been dried over potassium chloride for four times, dried by suction and kept in a desiccator containing phosphorus pentoxide at 65° C. for one hour with reducing the pressure by a vacuum pump which uses potassium hydroxide containing trap to obtain 17.03 g of crystalline 2-methyl-3-(trichlorogermyl) propionic acid:

1. waitat room temperature for 1.5 hour
2. filtrationThe precipitated crystal was filtered by suction
3. washwashed with 10 ml of n-hexane which
4. dry with materialhad been dried over potassium chloride for four times
5. customdried by suction
6. customkept in a desiccator
7. additioncontaining phosphorus pentoxide at 65° C. for one hour

ORD record

ord-b875d44972c24c0dbd5ac2ca3a939a65

Source dataset

uspto-grants-1991_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05071873