HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 3-(3-Chloro-benzyloxy)-phthalic acid dimethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-(Bromomethyl)-3-chlorobenzene | HCID 69838 | — |
| Reactant | Dimethyl 3-hydroxyphthalate | HCID 12223651 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 3-(3-Chloro-benzyloxy)-phthalic acid dimethyl ester | HCID 66906585 | 92% |
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 (2.1 g, 15.2 mmol) was added 3-chlorobenzyl bromide (1.0 mL, 7.6 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-(3-chloro-benzyloxy)-phthalic acid dimethyl ester (1.9 g, 92% yield). The product was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08614328B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-a65d166e9f84498eb74c8aeda819296a |
| Source note | uspto-grants-2013_12 |