HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 24766581, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Propargyl bromide | HCID 7842 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 24766692 | HCID 24766692 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 24766581 | HCID 24766581 | — |
Reaction Steps
1-O-(4,4′-dimethoxytrityl)-2-hydroxymethyl-2-methyl-1,3-propanediol 16 (620 mg, 1.47 mmol) was dissolved in anhydrous THF (6 mL) and sodium hydride (60% in oil, 590 mg, 14.7 mmol) was added. After 10 min stirring, propargyl bromide (80% in toluene, 650 mL, 5.9 mmol) was added and the mixture was stirred at RT for 1 h. Then CH2Cl2 was added (100 mL) and 2 mL of water. Organic layer was washed with water (2×100 mL) and dried over Na2SO4. After evaporation the residue was purified by flash chromatography using an increasing amount of ethyl acetate (10% to 50%) in cyclohexane containing 1% of triethylamine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08183355B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-b0f76fce7810447bb536447cfa7bc43e |
| Source note | uspto-grants-2012_05 |