HuagongsheHuagongshe Chemistry Print Report · For research reference only
O,O-Dipyridin-2-yl carbonothioate → Tert-butyl[(8-isothiocyanato-1,2,3,4-tetrahydronaphthalen-2-yl)oxy]dimethylsilane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | O,O-Dipyridin-2-yl carbonothioate | HCID 719784 | — |
| Reactant | 7-{[Tert-butyl(dimethyl)silyl]oxy}-5,6,7,8-tetrahydronaphthalen-1-amine | HCID 58734192 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Tert-butyl[(8-isothiocyanato-1,2,3,4-tetrahydronaphthalen-2-yl)oxy]dimethylsilane | HCID 75581950 | 72% |
Reaction Steps
A solution of the product of Example 18B, 2-(tert-butyldimethylsilyl)-ol (1.4 g, 5.07 mmol) and di-2-pyridyl thionocarbonate (1.07 g, 4.61 mmol) in 30 mL dichloromethane was stirred at room temperature overnight. The mixture was evaporated, then the residue was taken up in 2 mL dichloromethane and filtered through silica gel, eluting with 5% ethyl acetate-hexane. Evaporation of the filtrate afforded the product as a dark red oil (1.165 g, 72%). 1H NMR (DMSO-d6) δ 7.21 (m, 3H), 4.27 (m, 1H), 2.58-3.09 (m, 4H), 1.90 (m, 1H), 1.77 (m, 1H), 0.90 (s, 9H), 0.14 (s, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07504520B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-973473a85bce4c61ad758d2f94b5d00c |
| Source note | uspto-grants-2009_03 |