Diethyl Ether → Methyldichlorosilane

As control experiments, the ammonolysis of CH3SiCl3 alone was studied. Ammonolysis of this precursor in Et2O gave a 46% yield of soluble solid product, molecular weight 702 g/mol. ceramic yield (by TGA to 950° C.) 56%. A similar CH3SiCl3 /NH3 reaction in THF gave soluble solid product in 82% yield, molecular weight 672 g/mol, ceramic yield (by TGA) 69%. By proton NMR (CH3Si/NH integration), the Et2O product may be formulated as [CH3Si(NH)1.3 ]x, the THF product as [CH3Si(NH)1.6 ]x. (This is only a rough approximation because integration of the broad NH signals is rather inaccurate). The results of the coammonolyses of CH3SiHCl2 and CH3SiCl3 are given in Tables 4 and 5.

1. customceramic yield (by TGA to 950° C.) 56%
2. customgave soluble solid product in 82% yield, molecular weight 672 g/mol
3. customceramic yield (by TGA) 69%

ORD record

ord-db07fe4c714247efa1684627ab53a73e

Source dataset

uspto-grants-1988_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04720532