HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(4-Amino-3,5-dichlorophenyl)-2-bromoethan-1-one → HCID 23045282, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(4-Amino-3,5-dichlorophenyl)-2-bromoethan-1-one | HCID 3015897 | — |
| Reactant | HCID 23045285 | HCID 23045285 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23045282 | HCID 23045282 | 75.5% |
Reaction Steps
1-[4-Amino-3,5-dichlorophenyl]-2-bromoethanone (0.86 g), N-[3-[2-(3-phenylpropoxy)ethoxy]propyl]benzenemethanamine (1 g) and DEA (0.43 g) were stirred together in THF (30 ml) at room temperature under nitrogen for 22 h. The mixture was filtered and the filtrate evaporated in vacuo. The residue was dissolved in methanol (40 ml), treated portionwise with sodium borohydride (0.31 g) at 0° C. under nitrogen, stirred at room temperature under nitrogen for 2 h, diluted with water (150 ml) and extracted with ethyl acetate (2×150 ml). The dried extract was evaporated in vacuo to give an oil. Purification by FCC eluting with System F (1:1) gave the title compound (1.22 g) as an oil. T.l.c. (System F 1:1) Rf 0.19
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04937268 |
| Source dataset | uspto-grants-1990_06 |
| ORD ID | ord-db150cf2821e482b8e6b9c9c56628f90 |
| Source note | uspto-grants-1990_06 |