HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 3-Chloro-4-(2-acetoxyethoxy)benzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Acetoxy-2-bromoethane | HCID 13564 | — |
| Reactant | 3-Chloro-4-hydroxybenzaldehyde | HCID 17022 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 3-Chloro-4-(2-acetoxyethoxy)benzaldehyde | HCID 86611812 | 41.5% |
Reaction Steps
A mixture of 3-chloro-4-hydroxybenzaldehyde (10 g, 63.9 mmol), K2CO3 (26.5 g, 191.6 mmol) and 2-bromoethyl acetate (26.7 g, 159.7 mmol) in acetone (250 mL) is refluxed for 18 h before it is diluted with diethyl ether (200 mL) and washed with water (3×200 mL). The washings are extracted with diethyl ether (200 mL). The combined organic extracts are dried over MgSO4 and concentrated. The remaining residue is purified by column chromatography on silica gel eluting with heptane/EA 1:1 to afford the title compound (6.44 g) as colourless solid. 1H NMR (CDCl3): δ 9.85 (s, 1H9, 7.91 (d, J=1.8 Hz, 1H), 7.75 (dd, J=1.8, 8.2 Hz, 1H), 7.03 (d, J=8.8 Hz, 1H), 4.53-4.49 (m, 2H), 4.35-4.31 (m, 2H), 2.12 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | USRE045174E1 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-c930dde1d4144faab493bda65dd6931e |
| Source note | uspto-grants-2014_09 |