HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorotrimethylsilane → HCID 63911765, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | 4-Nitrobenzoyl chloride | HCID 8502 | — |
| Reactant | 2,6-Dimethylpiperazine | HCID 66056 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 63911765 | HCID 63911765 | 90% |
Reaction Steps
To a stirred solution of 2,6-di-methylpiperazine (LV, 5.0 g, 43.8 mmol) in dry THF (50 mL), maintained at room temperature under an argon atmosphere, was added a solution of 2.5 M n-BuLi in THF (38.54 mL, 96.36 mmol). After the mixture was stirred for 30 min at room temperature, trimethylsilyl chloride (5.5 mL, 43.8 mmol) was added and the reaction mixture stirred for 1 h before the addition of 4-nitrobenzoyl chloride (7.8 gm, 42.05 mmol). After 10 min, the reaction mixture was quenched with MeOH and the solvents were evaporated in vacuo. The residue was purified by silica gel column chromatography to provide product LVI (10.37 gm, 90% yield):
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08889667B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-e1beb29b379a4fedbd66379b565e3f7c |
| Source note | uspto-grants-2014_11 |