HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Iodide → 3-Iodo-2-propynyl butylcarbamate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Iodide | HCID 5238 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Chlorine | HCID 24526 | — |
| Edukt | 2-Propynyl butylcarbamate | HCID 10877354 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3-Iodo-2-propynyl butylcarbamate | HCID 62097 | 84,9% |
Reaktionsschritte
At 5° C., 19.0 g of propargyl butylcarbamate (0.122 mol), 12.2 g of sodium hydroxide (0.305 mol) and 18.5 g of sodium iodide (0.123 mol) are introduced as initial charge in 50 g of water and 48 g of methanol. Chlorine (11.7 g, 0.165 mmol) is then slowly introduced so that the temperature remains below 5° C. When the metered addition is complete, the mixture is stirred at this temperature for 1 h, then slowly heated to room temperature and stirred for 1 hour. After adding 100 g of water, the precipitated solid is isolated by filtration, washed with water and dried in vacuo. This gives 29.1 g of 3-iodo-2-propynyl N-butylcarbamate (purity: 94.7% (HPLC), polyiodized compounds: <0.1% (HPLC), yield: 80%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08748652B2 |
| Quelldatensatz | uspto-grants-2014_06 |
| ORD ID | ord-a1583321215b4e15adbd70039e6dd200 |
| Quellennotiz | uspto-grants-2014_06 |