Triethylamine → 2,6-Dichloro-4-isothiocyanatobenzonitrile
Reaktionsgleichung
[NH2:1][C:2]1[CH:9]=[C:8]([Cl:10])[C:5]([C:6]#[N:7])=[C:4]([Cl:11])[CH:3]=1.[C:12](Cl)(Cl)=[S:13].C(N(CC)CC)C>C1C=CC=CC=1>[Cl:11][C:4]1[CH:3]=[C:2]([N:1]=[C:12]=[S:13])[CH:9]=[C:8]([Cl:10])[C:5]=1[C:6]#[N:7]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A suspension of 4-amino-2,6-dichlorobenzonitrile (500 mg, 2.67 mmol, Eq: 1.00), thiophosgene (1.35 g, 900 μl, 11.7 mmol, Eq: 4.39), triethylamine (875 mg, 1.2 ml, 8.64 mmol, Eq: 3.23) in benzene (30 ml) was heated at reflux overnight. The brown reaction mixture was concentrated and chromatographed (80 g Analogix, 0 to 5% ethyl acetate/hexane) to give 436 mg (71%) of desired product as a light brown solid.
Aufarbeitung
- temperaturewas heated
- temperatureat reflux overnight
- concentrationThe brown reaction mixture was concentrated
- customchromatographed (80 g Analogix, 0 to 5% ethyl acetate/hexane)
Quellen und Nachweise
- ORD-Eintrag
- ord-c4b6bfec18f64e4893d1f23ecbb9a750
- Quelldatensatz
- uspto-grants-2016_08
- Patentnummer
- US09428469B2
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