HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 9885413, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Hydroxylamine | HCID 787 | — |
| Reactant | HCID 5063708 | HCID 5063708 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 9885413 | HCID 9885413 | 72.7% |
Reaction Steps
Freshly prepared hydroxylamine reagent (20 mL; 20 mmol) was added to ethyl 3-[(benzyl)-(4-methoxybenzenesulfonyl)-amino]-propionate (3.30 g; 8.8 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 (2×10 mL). The combined extracts were washed with saturated aqueous NaCl (1×10 mL), dried over MgSO4, and evaporated under reduced pressure to give a crude gum. Trituration with diethyl ether afforded 2.33 g (68%) of the title compound as an off-white solid. 300 MHz 1H-NMR (DMSO-d6): δ 2.06 (m, 2H), 3.25 (m, 2H), 3.87 (s, 3H), 4.33 (s, 2H), 7.16 (d, 2H), 7.20-7.42 (m, 5H), 7.80 (d, 2H), 8.70 (bs, 1H), 10.38 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06506936B1 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-8fd0c7312368434a87b5e35cca804fbb |
| Source note | uspto-grants-2003_01 |