HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(4-Amino-3,5-dichlorophenyl)-2-bromoethan-1-one → HCID 23045289, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(4-Amino-3,5-dichlorophenyl)-2-bromoethan-1-one | HCID 3015897 | — |
| Reactant | HCID 23045306 | HCID 23045306 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23045289 | HCID 23045289 | 70.9% |
Reaction Steps
1-[4-Amino-3,5-dichlorophenyl]-2-bromoethanone (0.95 g), N-[3-[2-(3-phenoxypropoxy)ethoxy]propyl]benzenemethanamine (1.15 g) and DEA (0.48 g) were stirred together in THF (35 ml) at room temperature under nitrogen for 7 h. The mixture was filtered and the filtrate evaporated in vacuo. The residue was dissolved in methanol (35 ml) and treated portionwise with sodium borohydride (0.34 g), at 0° C. under nitrogen, stirred at room temperature for 18 h, diluted with water (150 ml) and the solvent evaporated in vacuo. The residue was extracted with ethyl acetate (2×150 ml), dried and evaporated in vacuo to give an oil. Purification by FCC eluting with System H (95:5:1) gave the title compound (1.30 g) as an oil. T.l.c. (System H 90:10:1) Rf 0.39
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04937268 |
| Source dataset | uspto-grants-1990_06 |
| ORD ID | ord-99f4bd39155a4b3da82a905085e89576 |
| Source note | uspto-grants-1990_06 |