Acrylic Acid → Trichlorogermane propionic acid

An example of this alternative process follows. To a 50 L glass reactor was added successively: 7.2 Kg germanium tetrachloride, 5.3 Kg tetramethyl disiloxane, and 2.3y Kg of acrylic acid. The resulting mixture was stirred for 5 days forming TPA (trichlorogermane propionic acid) as a product. Volatile components were removed via vacuum distillation while the TPA product was heated to an internal temperature of 75° C.-80° C., where it was a homogeneous, clear and colorless viscous melt. Distillation is continued until no more distillate appears. The product was then cooled to ambient temperature yielding a white amorphous solid. To this was added 35 L of concentrated HCL. The resulting heterogeneous mixture was warmed to an internal temperature of 60° C.-70° C. and stirred for four hours and allowed to cool. The cooled mixture was extracted 3 times with 25 L of dichloromethane. Instead of removing all 75 L of the dichloromethane as in the previous examples, between about 50 L-70 L of the dichloromethane was removed with vacuum distillation at between about 25° C. to 40° C. to give a clear, colorless concentrated mixture. This concentrated mixture was poured into about 50 L of hexane at ambient temperature. Fine crystals of TPA appeared as a precipitant and the solution was let stand 4-8 hours. The solid is filtered. Then the solid is slowly added to 30 L of ammonium hydroxide (28-35%). To this, 21.6 L of 75% sulfuric acid was added over 2 hours with the temperature maintained below 25° C. The white solid was isolated via suction filtration, washed successively with 2×5.4 L acetone, and 2×5.4 L of diethyl ether, then the resulting brilliant white solid was air dried overnight to give a white solid. This white solid was then taken up in 9 L of hot water (~80° C.) and stirred for 2 hours, cooled and filtered to give a white solid, which was washed twice in 5.4 L water, then once with 5.4 L t-butyl methyl ether.

1. additionTo a 50 L glass reactor was added successively

ORD record

ord-d25d57c937d54908b324594695868440

Source dataset

uspto-grants-1997_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05703259