Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Phosgene | HCID 6371 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | N-Methylpentylamine | HCID 117479 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Lösungsmittel | Methylcyclohexane | HCID 7962 | — |
| Produkt | Methyl(pentyl)carbamyl chloride | HCID 15209943 | — |
Reaktionsschritte
Triethylamine (14 cc.) is added over the course of 8 minutes to a 2.5N solution (42 cc.) of phosgene in methylcyclohexane, cooled to -10° C., and a solution of N-methylpentylamine (13.7 cc.) in toluene (50 cc.) is then added whilst maintaining the temperature at -10° C. The mixture is stirred for 1 hour at +5° C. The insoluble material is then filtered off and washed with toluene (80 cc.). The organic solutions are dried over calcium chloride (10 g.). After filtration, the solvents are evaporated under reduced pressure (40 mm.Hg). The residue is distilled under reduced pressure to give N-methyl-N-pentylcarbamoyl chloride (5.6 g.), b.p. 120-125° C./40 mm.Hg.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04131674 |
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| Quelldatensatz | uspto-grants-1978_12 |
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| ORD ID | ord-a885dadfe7b7440faa0f634571ffd442 |
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| Quellennotiz | uspto-grants-1978_12 |
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