HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodoethane → 2,2-Diethylmalononitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodoethane | HCID 6340 | — |
| Reactant | Malononitrile | HCID 8010 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Product | 2,2-Diethylmalononitrile | HCID 2777231 | — |
Reaction Steps
Malononitrile (15.2 g) was mixed with TBAB (3.0 g, 4 mol %) and ethyl iodide (36.8 mL, 2 equiv.). After stirring for 30 minutes at room temperature, the mixture was cooled in an ice bath, KOtBu (51.6 g, 2 equiv.) was added portionwise, the ice bath was removed, and the mixture was stirred for 30 minutes at room temperature. Extraction with DCM/H2O, drying over Na2SO4 and evaporation under reduced pressure gave 40 grams of crude material, which was purified by flash chromatography eluting with DCM. This yielded 20.4 grams of an orange oil which solidified upon standing. 1H NMR (400 MHz, CDCl3) δ 1.29 (t, J=7.5 Hz, 6H), 2.00 (q, J=7.5 Hz, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07728018B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-70c666ce7b4a4ede94971688eaf95325 |
| Source note | uspto-grants-2010_06 |