HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → HCID 15728720, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Tributylstannane | HCID 5948 | — |
| Reactant | 1-(Chloromethoxy)-2-methoxyethane | HCID 77590 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Cyclohexane | HCID 8078 | — |
| Product | HCID 15728720 | HCID 15728720 | — |
Reaction Steps
Tributyltin hydride (2.69 ml, 0.01 mol) was added dropwise to a solution of lithium diisopropylamide (a 1.5M solution in cyclohexane; 6.7 ml, 0.01 mol) in tetrahydrofuran (20 ml) at 0° under argon. After 15 minutes, paraformaldehyde (300 mg, 0.01 mol) was added, followed by 2-methoxyethoxymethyl chloride (1.15 ml, 0.01 mol) after 3 hours. Stirring was continued at room temperature for 12 hours and the mixture was quenched with water. Extraction (ethyl ether) and evaporation of the dried (magnesium sulphate) extracts gave an oil, which was flash chromatographed on silica using 5% ethyl ether/petroleum ether. Fractions with Rf of about 0.24 on evaporation afforded the desired ether as a colorless oil (1.11 g, 27%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05045564 |
| Source dataset | uspto-grants-1991_09 |
| ORD ID | ord-6d340cf66f284cbc95e6c81f8deea1e2 |
| Source note | uspto-grants-1991_09 |