Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | HCID 58349500 | HCID 58349500 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58349438 | HCID 58349438 | — |
Reaction Steps
The product of step A (85 mg, 0.160 mmol) was dissolved in CH2Cl2 (15 mL) and triethylsilane (0.26 ml, 1.6 mmol) was added. The solution was cooled to −78° C., then BF3 gas was slowly bubbled through the solution until it was saturated (less than one minute, at the time fuming BF3 was observed from a small needle venting from the flask). The mixture was allowed to warm gradually to −20° C. When all starting material was consumed by LC/MS analysis, 1N HCl (aq) was added and the mixture was allowed to warm to room temperature. The mixture was extracted twice with CH2Cl2. The combined organic extracts were washed with water, dried over MgSO4, then concentrated. This afforded the title compound, which was used in the next step without purification: LC1 2.29 min. (M+H) 460.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08436015B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-edb37ceb0ffa48048c0b9349d66dd43c |
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| Source note | uspto-grants-2013_05 |
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