Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methyl Isocyanate | HCID 12228 | — |
| Edukt | 4-(2-Hydroxybenzylideneamino)-3,5-dimethylphenol | HCID 135689610 | — |
| Katalysator | Di-n-butyl diacetoxy tin | HCID 9798523 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 135689618 | HCID 135689618 | 68% |
Reaktionsschritte
To a 350 milliliter glass pressure bottle equipped with a magnetic stirrer was added 6.03 grams (0.025 moles) of 4-(2-hydroxybenzylideneamino)-3,5-dimethylphenol prepared in Part A, 1.71 grams (0.030 moles) of methyl isocyanate, 50 milliliters of ethyl acetate and 5 drops of dibutyltin diacetate. The resulting reaction mixture was stirred for 65 hours at room temperature and then washed twice with a 1% aqueous sodium bicarbonate solution followed by a single wash with saturated brine solution. After drying the reaction mixture over magnesium sulfate, it was collected by filtration and concentrated under reduced pressure to give a brown oil. The oil was triturated with hexane to give 5.21 grams (0.017 moles) of 4-(2-hydroxybenzylideneamino)-3,5-dimethylphenyl methylcarbamate in the form of a yellow solid having a melting point of 116°-118° C. and the following structural formula: ##STR8##
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04399148 |
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| Quelldatensatz | uspto-grants-1983_08 |
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| ORD ID | ord-73312b832c92420cb03e76f4873bfcc8 |
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| Quellennotiz | uspto-grants-1983_08 |
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