Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 1,2-Dichloroethane | HCID 11 | — |
| Edukt | Santonox | HCID 7308 | — |
| Edukt | m-Chloroperbenzoic acid | HCID 70297 | — |
| Edukt | N-(1-methylethyl)cinnamoylcarboxamide | HCID 3770630 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Produkt | HCID 13041334 | HCID 13041334 | — |
Reaktionsschritte
A mixture of N-(1-methylethyl)cinnamoylcarboxamide (18 g.), m-chloroperbenzoic acid (23.6 g.), 4,4'-thiobis(6-tert-butyl-m-cresol) (0.3 g.) and ethylene dichloride (250 ml.) was heated under gentle reflux for 1 hour, then chilled in ice. A precipitate (m-chlorobenzoic acid) was separated by filtration and washed with ethylene dichloride. The filtrate and washings were combined, and evaporated under reduced pressure on a rotary evaporator to give an amber oil. The oil was dissolved in chloroform (300 ml.) and the chloroform solution was washed with 5% aqueous sodium bicarbonate solution twice, then with saline. The chloroform solution was dried over magnesium sulfate, then evaporated under reduced pressure in a rotary evaporator to give an oil. The oil solidified on standing. The solid mass was recrystallized from ether giving 8.4 g. of product, m.p. 114°-115°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04401832 |
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| Quelldatensatz | uspto-grants-1983_08 |
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| ORD ID | ord-fbb28a7930114db6a365e29ed5593b54 |
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| Quellennotiz | uspto-grants-1983_08 |
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