HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 73691528, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 2,4-Difluorobenzaldehyde | HCID 73770 | — |
| Reactant | 2-(3-Methyl-3-nitrobutyl)-1,3-dioxolane | HCID 552563 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 73691528 | HCID 73691528 | 69% |
Reaction Steps
A suspension of 2,4-difluorobenzaldehyde (290.6 mg, 2.04 mmol), 2-(3-methyl-3-nitrobutyl)-1,3-dioxolane (776.8 mg, 4.11 mmol) and zinc (402.7 mg, 6.16 mmol) in ethanol (5 ml) was cooled to 0° C. in ice-water bath. Acetic acid (0.69 ml, 12.0 mmol) was added dropwise to the mixture. The mixture was gradually warmed to room temperature and stirred for 10 hours and let stand overnight. The mixture was filtered through Celite® bed and the filtrate was concentrated and purified by silica gel chromatography (hexane/ethyl acetate=4/1-1/1) to give the title compound (419.4 mg; 69%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06194461B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-5124b57524b047ebb2da08459d684bd9 |
| Source note | uspto-grants-2001_02 |