Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Trimethylsilyl triflate | HCID 65367 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 21874093 | HCID 21874093 | — |
| Reactant | HCID 59997913 | HCID 59997913 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10237940 | HCID 10237940 | — |
Reaction Steps
Trimethylsilyl trifluoromethanesulfonate (0.26 mL, 1.41 mmol) is added slowly over 15 min to a solution of the product from Step 7 (0.30 g, 0.71 mmol) and 2,6-lutidine (0.25 mL, 2.1 mmol) in dichloromethane (1.5 mL). The solution is stirred at room temperature for 1 h and then treated with methanol (1 mL). After 30 min, the solution is concentrated and redissolved in methanol (4 mL) and diisopropylethyl amine (0.38 mL, 2.1 mmol) is added. A solution of difluoro-thioacetic acid O-(3,3-diphenyl-propyl) ester (0.325 g, 0.71 mmol) in dichloromethane (0.5 mL) is then added and the solution stirred for 20 h at room temperature. The reaction mixture is then concentrated and the residue purified by column chromatography (0–1% MeOH-DCM) to provide the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07101874B2 |
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| Source dataset | uspto-grants-2006_09 |
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| ORD ID | ord-2f87fc6b8e0a41dfa1ef08a99eec0bc9 |
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| Source note | uspto-grants-2006_09 |
|---|