HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Chlorosulfonyl isocyanate → 6-methoxy-2-methyl-1H-indole-3-carbonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Chlorosulfonyl isocyanate | HCID 70918 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 6-methoxy-2-methyl-1H-indole | HCID 10844709 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 6-methoxy-2-methyl-1H-indole-3-carbonitrile | HCID 13904640 | 81% |
Reaktionsschritte
To a solution of 6-methoxy-2-methyl-1H-indole (3.9 g, 24 mmol) in acetonitrile (200 mL) and DMF (20 mL) is added dropwise a solution of ClSO2NCO (4 mL, 1.3 eq.) in acetonitrile (31 mL) at 0° C. After the addition, the mixture is stirred at room temperature for 3 h. Then it is poured into ice water and saturated NaHCO3 is added to it until it becomes basic. The aqueous phase is extracted with CH2Cl2 and then evaporated. The residue is purified with flash column chromatography on silica gel using EtOAc/petroleum ether (1/5) as eluent to yield 81% of 6-methoxy-2-methyl-1H-indole-3-carbonitrile.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07868037B2 |
| Quelldatensatz | uspto-grants-2011_01 |
| ORD ID | ord-a3b2adcd5e7a4039b8a70e9d60a9474a |
| Quellennotiz | uspto-grants-2011_01 |