HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorotrimethylsilane → N,N'-Dimethyl-N,N'-bis(trimethylsilyl)urea
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | N,N'-Dimethylurea | HCID 7293 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | N,N'-Dimethyl-N,N'-bis(trimethylsilyl)urea | HCID 12479153 | — |
Reaction Steps
1,3-dimethylurea (44.0 g, 0.5 mole) and triethylamine (250 mls) were charged to a stirred reaction vessel purged with dry nitrogen. The mixture was stirred for 5 minutes and then chlorotrimethylsilane (167.5 mls, 1.32 moles) was added resulting in the formation of a white precipitate. The resulting reaction mixture was stirred for a further 24 hours at ambient temperature after which it was filtered under a nitrogen atmosphere. The filter cake was washed with dry toluene and the combined organics filtrate was distilled at atmospheric pressure under a nitrogen atmosphere. The residual organics were subjected to fractional distillation at a pressure of 8 mmHg. The fraction distilling at 86° to 88° C. was the required initiator.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05196489 |
| Source dataset | uspto-grants-1993_03 |
| ORD ID | ord-51c3e08149ca45bf8c72b0f2bd997f47 |
| Source note | uspto-grants-1993_03 |