Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Hydroxybenzophenone | HCID 14347 | — |
| Reactant | 3-Chloropropionyl chloride | HCID 69364 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | HCID 59609091 | HCID 59609091 | — |
Reaction Steps
6.7 g (35 mmol) of 4-hydroxy-benzophenone was dissolved in 100 ml methyl ethyl ketone. 4.2 g (42 mmol) triethyl amine was added and the mixture was cooled to −10° C. 5.3 g (42 mmol) 3-chloro-propionyl chloride was added drop wise, while the temperature was kept below −5° C. The reaction was allowed to continue for 30 minutes at 0° C. and 3 hours at room temperature. The precipitated salts were removed by filtration and the solvent was evaporated under reduced pressure. 3-Chloro-propionic acid 4-benzoylphenyl ester was isolated by preparative column chromatography on a Prochrom LC80 column, using n-hexane/ethylacetate 75/25 as eluent at a flow rate of 150 ml/min and Kromasil 60A 10 micron as silica. 1.2 g of 3-chloro-propionic acid 4-benzoylphenyl ester was isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08664431B2 |
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| Source dataset | uspto-grants-2014_03 |
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| ORD ID | ord-7ac7db95eda0472a88c547ea754a6033 |
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| Source note | uspto-grants-2014_03 |
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