HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 58574583, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 2-Amino-4-bromobenzoic acid | HCID 88691 | — |
| Reactant | HCID 58574408 | HCID 58574408 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58574583 | HCID 58574583 | — |
Reaction Steps
A solution of 2-amino-4-bromobenzoic acid (2.8 g, 13.1 mmol, 1.1 equiv), (9H-fluoren-9-yl)methyl 2-methyl-5-oxopiperazine-1-carboxylate (4 g, 11.9 mmol, 1 equiv), and phosphoryl trichloride (4 mL) in 1,4-dioxane (100 mL) was stirred at 80° C. for two hours. After it was cooled to room temperature, the reaction mixture was quenched with water and extracted with ethyl acetate (3×100 mL). The combined organic layers were dried over Na2SO4. After filtration and concentration, the residue was purified by silica gel chromatography to give the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772301B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-15f57db3de43446ca6ea340f8f9b62c4 |
| Source note | uspto-grants-2014_07 |