HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 69655025, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 21021937 | HCID 21021937 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 69655025 | HCID 69655025 | 94.6% |
Reaction Steps
A solution of 0.10 g (0.2 mmol) of (E)-3-(4-{4-[(2R)-2-hydroxy-2-(4-hydroxy-3-methanesulfonylamino-phenyl)-ethylamino]-piperidin-1-yl}-phenyl)-acrylic acid ethyl ester (which was obtained in Example 183) in ethanol (3 mL) was treated with 3 mL of 1 N NaOH. After 18 h at room temperature, the mixture was acidified with acetic acid. The resulting suspension was filtered and the precipitate was washed with water, and dried in vacuo to give 0.09 g of a tan solid; m.p. 220° C.; 1H NMR (DMSO-d6) δ 1.20–1.40 (m, 2 H), 1.80–1.95 (m, 2 H), 2.57–2.95 (m, 5 H), 2.92 (t, 3 H), 3.74–3.82 (m, 2 H), 4.48–4.52 (m, 1 H), 6.22 (s, 1 H), 6.27 (s, 1 H), 6.81–7.03 (m, 4 H), 7.18 (d, 1 H), 7.42–7.49 (m, 3 H)); MS (ES) m/z: 476.0 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07022716B2 |
| Source dataset | uspto-grants-2006_04 |
| ORD ID | ord-7ba43c1d82ac448cb0d224f2e64bdcb4 |
| Source note | uspto-grants-2006_04 |