Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroethane | HCID 6337 | — |
| Reactant | 2,4,6-Trimethylbenzoyl chloride | HCID 97038 | — |
| Reactant | HCID 18983532 | HCID 18983532 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 18983517 | HCID 18983517 | 81% |
Reaction Steps
96.4 g (0.528 mol) of 2,4,6-trimethylbenzoyl chloride and 1.2 g of triethylamine were heated to 115° C. and 65 g (0.264 mol) of monoethyl monophenyl phenylphosphonite were added dropwise in 75 minutes under a nitrogen atmosphere and with vigorous stirring. Ethyl chloride was given off as gas and was condensed in a downstream cold trap. The mixture was then further stirred for 2 hours at 115° C. and simultaneously a relatively strong nitrogen stream was passed through the apparatus. In total, at the end of the reaction 16 g (94% of theory) of ethyl chloride were situated in the cold trap. The excess 2,4,6-trimethylbenzoylchloride was then distilled off at 1 mbar and the residue was distilled with the aid of a thin-film evaporator (bath temperature: 230° C.; 0.3 mbar). 78 g were obtained. The yield was 81% of theory.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05498741 |
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| Source dataset | uspto-grants-1996_03 |
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| ORD ID | ord-e2e7e1fe102c44e6851e8b9034182809 |
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| Source note | uspto-grants-1996_03 |
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