HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → HCID 11562119, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | HCID 68820138 | HCID 68820138 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 11562119 | HCID 11562119 | 27% |
Reaction Steps
The objective compound was prepared by the same procedure for the example 1, using a 3,5-dibromo-2-[2-(4-methoxy-3-nitro-phenyl)-propionylamino]-benzoic acid methyl ester (0.65 g, 1.26 mmol) and LiHMDS (3.78 mmol, 1M solution in THF). After normal workup, the objective compound (160 mg, 27%) was obtained as white solid by a flash column chromatography (n-hexane:EtOAc=2:1): 1H NMR (200 MHz, DMSO-d6) δ 1.68 (s, 3H, CH3), 3.87 (s, 3H, OCH3), 7.32 (d, J=9.0 Hz, 1H, ArH), 7.43 (dd, J=8.8, 2.4 Hz, 1H, ArH), 7.69 (d, J=2.4 Hz, 1H, ArH), 7.84 (d, J=2.6 Hz, 1H, ArH), 8.12 (d, J=2.6 Hz, 1H, ArH); MS(EI) m/e 482 [M+], 277, 207, 102 ; HRMS m/e cacld. for C17H12N2O5Br2 481.9113, found 481.9122.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07592457B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-4e0f4eb1b54d448a9996d9e9a194473b |
| Source note | uspto-grants-2009_09 |