Reaktion #1286191

Reaktionsgleichung

triethylamine

2-aminobenzophenone

(methylthio)acetonitrile

t-butyloxychloride

→

dark oil

Ausbeute 106.7%

2-Amino-3-benzoyl-α-(methylthio)benzeneacetonitrile

Ausbeute 106.7%

Lösungsmittel

methylene dichloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigedid not exceed -64° C
2. 2
   Temperaturto warm to ambient temperature
3. 3
   SonstigeThe solution obtained
4. 4
   Waschenwas washed twice with water
5. 5
   Trocknendried over sodium sulphate
6. 6
   Einengenconcentrated

Vorschrift

To a slurry of 29.6 g (0.15 mole) of 2-aminobenzophenone and 13.1 g (0.15 mole) of (methylthio)acetonitrile in 400 ml of methylene dichloride at a temperature of -68° C. was added dropwise 16.8 g (0.155 mole) of t-butyloxychloride at a rate to ensure that the reaction temperature did not exceed -64° C. The resulting solution was stirred at -69° C. for one hour, treated with 15.7 g (0.155 mole) of triethylamine and allowed to warm to ambient temperature. The solution obtained was washed twice with water, dried over sodium sulphate, and concentrated to give 45.2 g of a dark oil as the residue. This residue was chromatographed on 1 kg of silica gel to yield 22.5 g (53%) of the title compound as tan crystals, m.p. 107°-108° C.

Quelle