HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → Butanoic acid, 2-hydroxy-2-(trifluoromethyl)-, ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Ethyl 3,3,3-trifluoro-2-oxopropanoate | HCID 2737239 | — |
| Reactant | HCID 178461630 | HCID 178461630 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | Butanoic acid, 2-hydroxy-2-(trifluoromethyl)-, ethyl ester | HCID 57437841 | — |
Reaction Steps
To a −78° C. solution of ethyl trifluoropyruvate (129.0 g 758 mmol) in ether was added dropwise within 90 min a solution of EtMgBr 3.0 M in ether (252 mL). The solution was brought over one 1 h to ca. −10° C. and poured over 2 L of saturated NH4Cl. The layers were separated and the aqueous phase extracted with ether (3×500 mL). The organic phases were combined, dried over MgSO4 and the solvent removed. Distillation at 50-65° C. (30 mm Hg) gave the title compound. 1H NMR (400 MHz, acetone-d6): δ 5.4 (s, 1H), 4.35 (q, 2H), 2.07 (m, 1H), 1.83 (m, 1H), 1.3 (t, 3H) and 0.93 (t, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07553973B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-6f8b6da1c94d4267ac1cf42488feda7f |
| Source note | uspto-grants-2009_06 |