HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Chloro-4-(chloromethyl)benzene → 3-(4-Chloro-benzyloxy)-phthalic acid dimethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Chloro-4-(chloromethyl)benzene | HCID 7723 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Dimethyl 3-hydroxyphthalate | HCID 12223651 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 3-(4-Chloro-benzyloxy)-phthalic acid dimethyl ester | HCID 66906746 | 109.1% |
Reaction Steps
To a stirred suspension of 3-hydroxyphthalic acid dimethyl ester (1.3 g, 6.3 mmol) in acetone (20 mL) and potassium carbonate (2.6 g, 19 mmol) was added 4-chlorobenzyl chloride (1.1 g, 6.6 mmol) and refluxed overnight. The solvent was evaporated and the residue was partitioned between water (100 mL) and ethyl acetate (150 mL) and washed with water (2×100 mL). The combined organic phases was dried, concentrated and purified by flash column chromatography (EtOAc/Hexane) to give 3-(4-chloro-benzyloxy)-phthalic acid dimethyl ester (2.3 g, 110% crude yield). The product was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181216B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-183ee1d1e2ee4875bd427905de683bfc |
| Source note | uspto-grants-2015_11 |