Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 11730256 | HCID 11730256 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Product | HCID 11144234 | HCID 11144234 | — |
Reaction Steps
A solution of 297 mg (0.642 mmol) of 62 crude in 10 mL of 2-methoxyethyl ether was stirred and heated at 162° C. for 15 min. The reaction mixture was allowed to cool to rt, poured into H2O (100 mL) and extracted with EtOAc (3×, 70 mL). Combined organic extracts were washed with 10% Na2S2O5 and concentrated in vacuo giving a yellow oil which was used without purification in the next step. Data for 63: TLC, T-3, Rf 0.58; 1H NMR (400 MHz, CDCl3) δ 1.01 (s, 3H, H-18), 5.04 (s, 2H, benzylic-H), 6.72 (d, 1H, J=2.6 Hz, H-4), 6.81 (dd, 1H, J=8.5, 2.6 Hz, H-2), 7.22 (d, 1H, J=8.5 Hz, H-1), 7.30–7.45 (m, 5H, Ar—H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07015211B2 |
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| Source dataset | uspto-grants-2006_03 |
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| ORD ID | ord-daf55640446e46cbbbcf91462d3f622b |
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| Source note | uspto-grants-2006_03 |
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