HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 18678912, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Hydroxylamine | HCID 787 | — |
| Reactant | HCID 18678882 | HCID 18678882 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 18678912 | HCID 18678912 | 65% |
Reaction Steps
Freshly prepared hydroxylamine reagent (20 mL; 20 mmol) was added to ethyl 3-[(phenethyl)-(4-methoxy-benzenesulfonyl)-amino]-propionate (3.30 g; 9.1 mmol) and the resulting mixture stirred for 18 h at room temperature. The mixture was poured into 1 N HCl (100 mL) and extracted with CH2Cl2 (2×100 mL). The combined extracts were washed with saturated aqueous NaCl (1×100 mL), dried over MgSO4, and evaporated under reduced pressure to give a crude gum. Trituration with diethyl ether afforded 2.23 g (65%) of the title compound as an off-white solid. 300 MHz 1H-NMR (DMSO-d6): δ 2.23 (t, 2H), 2.74 (m, 2H), 3.23 (m, 2H), 3.34 (m, 2H), 3.83 (s, 3H), 7.11 (d, 2H), 7.15-7.34 (m, 5H), 7.72 (d, 2H), 8.78 (s, 1H), 10.50 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06506936B1 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-a187da58c8e843a6b42197dd35902d70 |
| Source note | uspto-grants-2003_01 |