Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroethane | HCID 6337 | — |
| Reactant | 2,4,6-Trimethylbenzoyl chloride | HCID 97038 | — |
| Reactant | HCID 10935541 | HCID 10935541 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 18983522 | HCID 18983522 | 87% |
Reaction Steps
69.7 g (0.382 mol) of 2,4,6-trimethylbenzoyl chloride and 0.9 g of triethylamine were heated under a nitrogen atmosphere to 115° C. and 57.8 g (0.191 mol) of monoethyl mono-2-tert-butylphenyl phenylphosphonite were added dropwise in one hour with stirring. Ethyl chloride was given off as a gas and was condensed in a downstream cold trap. The mixture was further stirred for 2 hours. In total, 11.7 g of ethyl chloride (95% of theory) condensed. After distilling off the excess acid chloride, the residue was distilled with the aid of a thin-film evaporator (bath temperature: 270° C.; 0.4 mbar). 70 g were obtained. The product was brought to crystallization from concentrated acetone solution, melting point: 76°-79° C. The yield was 87% 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-bec4990568654214ab7d93dfb6010d15 |
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| Source note | uspto-grants-1996_03 |
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