HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → 1,3-Diethyl 2-[2'-chloro-4'-(trifluoromethyl) [1,1'-biphenyl]-3-yl]propanedioate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ethyl 2'-chloro-4'-(trifluoromethyl)[1,1'-biphenyl]-3-acetate | HCID 66973842 | — |
| Solvent | Diethyl Carbonate | HCID 7766 | — |
| Product | 1,3-Diethyl 2-[2'-chloro-4'-(trifluoromethyl) [1,1'-biphenyl]-3-yl]propanedioate | HCID 66973616 | — |
Reaction Steps
NaH (1.2 g, 60% dispersion in mineral oil) was added to the product of Step A dissolved in diethyl carbonate (10 mL). The reaction mixture was stirred overnight and then cautiously quenched by careful addition to saturated aqueous ammonium chloride solution. The quenched reaction mixture was extracted with ethyl acetate, and the separated orgranic phase was dried and concentrated under vacuum to yield 2.1 g of the title compound containing approximately 30% diethyl carbonate. 1H NMR (CDCl3) δ 7.74 (s, 1H), 7.57 (d, 1H), 7.35-7.55 (m, 5H), 4.57 (s, 1H) 4.19 (q, 4H), 1.29 (t, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09314025B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-90074f2421644f42b679957fed90ad88 |
| Source note | uspto-grants-2016_04 |