Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | HCID 18921935 | HCID 18921935 | — |
| Reactant | HCID 66915646 | HCID 66915646 | — |
| Catalyst | Titanium Tetrachloride | HCID 24193 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66915588 | HCID 66915588 | — |
Reaction Steps
A solution of 2.61 mmol of trimethylsilyloxy trifluoromethanesulphonate in 1 ml of dichloro-methane at 0° C. is admixed with a solution of 1.27 mmol of titanium tetrachloride in 1.5 ml of dichloromethane. The mixture is stirred at room temperature for 4 hours and then cooled to 0° C. A solution of 0.83 mmol of 7-methoxy-6′,7′-dihydro-5′H-spiro[chromene-4,8′-imidazo[1,5-a]pyridin]-2(3H)-one and 4.17 mmol of triethylsilane in 2 ml of dichloromethane is added and the reaction mixture is stirred at room temperature for 20 hours. The reaction mixture is poured into ice-water and extracted with ethyl acetate (2×). The combined organic phases are washed with water and brine, dried with sodium sulphate and evaporated. From the residue the title compound is identified by means of flash chromatography (SiO2 60F) on the basis of the Rf value.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08071774B2 |
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| Source dataset | uspto-grants-2011_12 |
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| ORD ID | ord-609d2b85025e42928b1b8d673e934751 |
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| Source note | uspto-grants-2011_12 |
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