Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | Tris(trimethylsilyl)silane | HCID 123134 | — |
| Reactant | HCID 58119785 | HCID 58119785 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 58119773 | HCID 58119773 | — |
Reaction Steps
10 mg 8-(tert-Butyl-dimethyl-silanyloxy)-9-cyclopentyl-3-iodomethyl-3,6,6-trimethyl-1-(4-trifluoromethyl-phenyl)-1,3,5,6,7,8-hexahydro-furo[3,4-b]quinoline (example XXI) are dissolved in 1 ml toluene and mixed successively under argon with 300 μl tris-trimethylsilyl-silane and 1 mg azo-bis-isobutyro-nitrile. The reaction mixture is heated for 4 hours to 110° C. and for 12 hours at room temperature. After addition of 1 ml methanol the solvents are evaporated in vacuo and the residue is partitioned between water and ethylacetate. The aqueous phase is extracted twice with ethylacetate and the combined organic phases are washed with brine. After drying with magnesium sulphate the solvents are evaporated in vacuo. The crude product thus obtained is directly submitted to the next step (example 1 (4)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08703793B2 |
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| Source dataset | uspto-grants-2014_04 |
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| ORD ID | ord-e90bd49776a747d0b04fd16228534d2e |
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| Source note | uspto-grants-2014_04 |
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