HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorotrimethylsilane → HCID 67955212, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 1,2-Difluorobenzene | HCID 9706 | — |
| Reactant | tert-Butyl methyl ether | HCID 15413 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67955212 | HCID 67955212 | — |
Reaction Steps
625 ml (1 mol) of 1.6 M BuLi are added dropwise at −78° C. to a solution of 114 g (1 ml) of 1,2-difluorobenzene in 11 of dry tetrahydrofuran. After 1 hour, 140 ml (120 g, 1.1 mol) of trimethylsilyl chloride are slowly added dropwise at −78° C. The mixture is allowed to warm to room temperature overnight, and then 200 ml of methyl ter-butyl ether and 200 ml of water are added. The organic phase is washed with water (2×100 ml) and sat. NaCl (1×100 ml) and dried using magnesium sulfate, and the solvent is removed under reduced pressure. 170 g (91%) of 5 distil over from the residue at from 100 to 102° C./70 mbar.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08350100B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-7dc5faf8fffa457bbb6562012632b700 |
| Source note | uspto-grants-2013_01 |