HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 12015903, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Magnesium perchlorate | HCID 24840 | — |
| Reactant | Azidotrimethylsilane | HCID 78378 | — |
| Reactant | HCID 12015902 | HCID 12015902 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 12015903 | HCID 12015903 | — |
Reaction Steps
To a solution of the compound obtained in Step C (3.52 g/14.65 mmol) in 50 ml of 1,2-dichloroethane there are added dropwise trimethylsilyl azide (TMSN3), and then 0.326 g (1.46 mmol) of magnesium perchlorate (Mg(ClO4)2), and the whole is stirred at room temperature overnight. Hydrolysis is then carried out using H2O, followed by extraction with AcOEt; the organic phases are then combined, washed with a saturated NaCl solution, dried over MgSO4 and concentrated to dryness. The yellow oil so obtained is chromatographed over a column of silica gel (cyclohexane, 2% AcOEt) to yield the title product in the form of a translucent oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06638962B2 |
| Source dataset | uspto-grants-2003_10 |
| ORD ID | ord-89cb1e43fb5640e293885fff355101e3 |
| Source note | uspto-grants-2003_10 |