HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Methyl 2-chloro-4-(hydroxymethyl)benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 1,4-Benzenedicarboxylic acid, 2-chloro-, 1-methyl ester | HCID 21276533 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Methyl 2-chloro-4-(hydroxymethyl)benzoate | HCID 19780655 | 99.1% |
Reaction Steps
Borane-methyl sulfide complex (10 M; 10 mL, 100 mmol) was added to a solution of 2-chloro-1,4-benzenedicarboxylic acid, 1-methyl ester (Example 1; 11.98 g, 55.8 mmol) in tetrahydrofuran (100 mL). The solution was heated at reflux for 2 h and then allowed to stand at room temperature overnight. It was poured into water and ethyl acetate (200 mL each). The layers were separated and the aqueous layer was extracted with ethyl acetate (100 mL). The combined organic layers were washed with brine (200 mL), dried (MgSO4), filtered, and evaporated to give 2-chloro-4-(hydroxymethyl)benzoic acid, methyl ester (11.09 g, 99%) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06803384B2 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-81e3bf505df149e29f8c9a6753e74dee |
| Source note | uspto-grants-2004_10 |