HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 178445686, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 178497907 | HCID 178497907 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | HCID 178445686 | HCID 178445686 | — |
Reaction Steps
To a solution of the intermediate from step E (isomer A, 0.3 g, 0.56 mmol) in 10 ml of THF/MeOH was added 5 N NaOH (1 mL). The reaction was stirred at room temperature for 2 hours and concentrated in vacuo. The residue was acidified with 1N HCl (10 ml). The resulting mixture was extracted with ethyl acetate, dried over anhydrous Na2SO4 filtered and concentrated in vacuo. This material was used in the next step without any further purification. 1H NMR (CD3OD, 500 MHz): 8.26 (d, J=2.1 Hz, 1H), 7.96 (d, J=8.3 Hz, 1H), 7.59 (dd, J=6.6, 8.9 Hz, 1H), 7.31 (d, J=8.3 Hz, 1H), 7.17 (s, 1H), 5.83 (s, 2H), 3.7 (m, 1H), 1.95 (d, J=10.1 Hz, 1H), 1.86 (d, J=10.3 Hz, 1H), 1.3 (m, 2H), 1.15 (m, 2H), 1.0 (m, 1H), 0.88 (s, 9H). LC-MS: 4.25 min; (M+H)=514.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07649009B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-d6814dc929b841769a4864b53d974716 |
| Source note | uspto-grants-2010_01 |