HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 3-(4-[2-(6,11-Dihydrodibenzo[b,e]thiepin-11-yloxy)-ethoxy]-phenyl)-2-ethoxy-propionic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 3-(4-[2-(6,11-Dihydrodibenzo[b,e]thiepin-11-yloxy)-ethoxy]-phenyl)-2-ethoxy-propionic acid ethyl ester | HCID 9891844 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 3-(4-[2-(6,11-Dihydrodibenzo[b,e]thiepin-11-yloxy)-ethoxy]-phenyl)-2-ethoxy-propionic acid | HCID 9934171 | 62% |
Reaction Steps
3-(4-[2-(6,11-Dihydrodibenzo[b,e]thiepin-11-yloxy)-ethoxy]-phenyl)-2-ethoxy-propionic acid ethyl ester (example 2) (220 mg, 0.44 mmol) in ethanol (5 mL) was added NaOH 1N (0.9 mL, 0.9 mmol). The mixture was stirred at room temperature for 16 h. The ethanol was evaporated of and pH adjusted with HCl 1N to pH 1. After extraction with dichloromethane the product was purified by chromatography, using dichloromethane/methanol (9:1) as eluent, to give 126 mg (62%) of the title compound: 1H NMR (300 MHz, CDCl3) δ1.15 (t, 3H), 2.85-3.10 (m, 2H), 3.32-3.42 (m, 1H), 3.52-3.65 (m, 1H), 2.85 (t, 2H), 3.95-4.05 (m, 1H), 4.10-4.22 (m, 2H), 4.5-5.1 (bs, 1H), 5.60-5.75 (bs, 1H), 6.82 (d, 2H), 7.05-7.50 (m, 10H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06602901B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-8aa5539f40424ae69b19a7bcb4254c77 |
| Source note | uspto-grants-2003_08 |