HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Lutidine → HCID 86755965, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Dabco | HCID 9237 | — |
| Reactant | Trifluoromethanesulfonate | HCID 2758875 | — |
| Reactant | HCID 10582768 | HCID 10582768 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86755965 | HCID 86755965 | 100.5% |
Reaction Steps
(R)-(−)-3-azido-2-methylpropanol (0.64 g, 5.56 mmol) was dissolved in CH2Cl2 (40 mL). 2,6-lutidine (1.9 mL, 16.3 mmol) was added at −20° C. followed by adding trifalic anhydride (1.4 mL, 8.32 mmol). The mixture was kept in −20° C. for 40 min, diluted with CH2Cl2, washed with water, 0.1 N HCl aqueous solution, water and brine, dried over Na2SO4 and concentrated to give the trifalte (1.33 g). The triflate (0.7 g, 2.83 mmol) was reacted with 1,4-diazabicyclo[2.2.2]octane (0.31 g, 2.77 mmol) in CH3CN for 3 hrs. The solvent was removed and the residue was dried under vacuum to give the product (1.0 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06399597B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-3fa9e5ce704c44a1a8b201f346e5b956 |
| Source note | uspto-grants-2002_06 |