HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → 1,3-Dioxolane-2-propionaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 2-(2-Bromoethyl)-1,3-dioxolane | HCID 87776 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1,3-Dioxolane-2-propionaldehyde | HCID 3661214 | 28% |
Reaction Steps
To the solution of 2-(2-bromoethyl)-1,3-dioxolane (10 g, 55.2 mmol) in THF (50 mL) was added magnesium (1.6 g, 66.3 mmol) and trace amount of I2 as initiator. The reaction mixture was stirred at rt for 2 hrs. After cooling to −78° C., the mixture was quenched with dry DMF (1.39 g, 66.3 mmol) and kept at −78° C. for 2 hrs. After dilution with H2O the reaction mixture was extracted with CH2Cl2 (2×), followed by distillation (45-55° C. @ 8 mmHg) to afford 2 g (28%) of the title compound. MS (DCI/NH4+) m/z 131 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835475B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-cb2e95cbfab14f60ac1af2e9fbf5e1e1 |
| Source note | uspto-grants-2014_09 |