HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 67099311, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Phosphorus oxide (P4O10) | HCID 14812 | — |
| Reactant | HCID 67099610 | HCID 67099610 | — |
| Product | HCID 67099311 | HCID 67099311 | 46.5% |
Reaction Steps
H2SO4 (40 mL, 473 mmol) was cooled to 0° C. and treated with P2O5 (15 g, 106 mmol). The mixture was brought to room temperature and added to diethyl 2-(2-(3-chlorophenyl)-2-methylbutanoyl)malonate (7.67 g, 22 mmol). The reaction mixture was then stirred for 1.5 hours. Ice (H2O) was added, and the aqueous mixture was extracted with EtOAc (3×). The combined organic layers were washed with water (2×) and brine, dried (MgSO4), and concentrated in vacuo to give the crude compound as an orange oil. The crude oil was purified by silica flash chromatography (0-100% DCM/hexane) to give the desired compound as a yellow solid (3.16 g). MS (m/e)=309.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928139B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-ea7fe8ad95194750b3eea67a871bef84 |
| Source note | uspto-grants-2011_04 |