HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86703134, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Propylphosphoric anhydride | HCID 16167369 | — |
| Reactant | HCID 86703135 | HCID 86703135 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86703134 | HCID 86703134 | — |
Reaction Steps
A solution of propylphosphonic anhydride (T3P/PPA) (50% in EtOAc) (7.13 mmol) was added dropwise to a solution of 4-chloro-2-[6-(4-chloro-phenyl)-1-isopropyl-4-oxo-4,6-dihydro-1H-pyrrolo[3,4-b]pyrrol-5-yl]benzamide (Step AB2) (3.10 mmol) and Et3N (3.41 mmol) in EtOAc (25 mL) at 45° C. After 23 h, the reaction mixture was cooled to rt and partitioned between EtOAc and H2O. The organice phase was successively washed with a saturated aqueous solution of NaHCO3, water and brine, dried (Na2SO4), filtered and concentrated. The residue was purified using a RediSep® silica gel column to afford the title compound as a white solid. tR: 4.97 min (HPLC 1); ESI-MS: tR=1.19 min, [M+H]+ 410/412/414 (LC-MS 1); TLC: Rf=0.16 (1:3 EtOAc/heptanes).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09365576B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-6db4354f2d404e009abdf442b0e75c18 |
| Source note | uspto-grants-2016_06 |