HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86660872, compound → HCID 66656204, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86660872 | HCID 86660872 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 66656204 | HCID 66656204 | 78.1% |
Reaction Steps
Intermediate 16A (1.9 g, 5.93 mmol) was dissolved in a 4.0 M solution of HCl in MeOH (30 mL) and the reaction mixture was stirred at RT overnight. The mixture was concentrated and the residue was dissolved in water. The aqueous solution was basified to pH=10 with aqueous NaOH (1.0 M) and then extracted with DCM (4×30 mL). The combined organic phases were filtered through a phase separator and the solvent was removed by evaporation. There was obtained 1.02 g (78%) of 16B as a colorless oil. 1H NMR (500 MHz, CDCl3): δ 2.21 (s, 6H), 2.33 (s, 3H), 3.30 (s, 2H), 3.73-3.84 (m, 2H), 3.85-3.96 (m, 2H), 4.91-5.03 (m, 1H), 6.52 (d, 1H), 6.58 (s, 1H), 7.11 (d, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08546375B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-914cfa2e04b647d39c9a2fb10cf28143 |
| Source note | uspto-grants-2013_10 |