HuagongsheHuagongshe Chemistry Print Report · For research reference only
Solketal → HCID 67254478, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Solketal | HCID 7528 | — |
| Reactant | Methyl cyanoacetate | HCID 7747 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Product | HCID 67254478 | HCID 67254478 | 23% |
Reaction Steps
A mixture of methyl cyanoacetate (1.3 ml, 15×10−3 mol), of solketal (1.25 ml, 10×10−3 mol) and of DMAP (2.7 mg, 0.03 equiv.) is heated at reflux with stirring for 30 hours in a reactor rendered inert with nitrogen. After cooling, the solvent is evaporated under vacuum and the brown oil obtained is chromatographed on a silica column (gradient of eluents: heptane/EtOAc from 90:10 to 80:20). 423 mg (yield: 23%) of the pure fractions of (2,2-dimethyl-1,3-dioxolan-4-yl)methyl cyanoacetate are thus obtained in the form of a yellow oil used as is in the following stage.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08961941B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-ebb0052f06d6412f905c044545d6ed17 |
| Source note | uspto-grants-2015_02 |