HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 43390057, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Amino-1-propanol | HCID 9086 | — |
| Reactant | Benzeneacetyl chloride, 4-nitro- | HCID 6452210 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 43390057 | HCID 43390057 | 11.4% |
Reaction Steps
To a stirred solution of 3-hydroxypropylamine (507 mg, 6.76 mmol) and triethylamine (1.88 mL, 0.013 mol) in DCM (10 mL) at 0° C. was added (4-nitro-phenyl)-acetyl chloride (1.35 g, 6.76 mmol) in DCM (10 mL) dropwise. The dark red solution was allowed to warm to room temperature and then poured into water (50 mL). The layers were separated and the organic layer was dried (Na2SO4) and concentrated in vacuo. The crude material was purified by preparative thin layer chromatography (TLC) (5%-MeOH—CHCl3) to afford 183 mg (11%) of the title compound as a solid. 1H-NMR (CDCl3; 400 MHz): δ 8.12 (d, 2H, J=8.7 Hz), 7.39 (d, 1H, J=8.7 Hz), 6.09 (br s, 1H), 3.58 (s, 2H), 3.57-3.54 (m, 2H), 3.40 (br s, 1H), 3.36-3.31 (m, 2H), 1.63-1.57 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09221797B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-f60bb0414b7b4ea2834b3648b48d51c2 |
| Source note | uspto-grants-2015_12 |