Reaktion #1286192

Reaktionsgleichung

4'-chloro-2-aminobenzophenone

methylthioacetonitrile

tert. butyloxychloride

→

title compound

Ausbeute 68.0%

2-Amino-3-(4-chlorobenzoyl)-α-(methylthio)benzeneacetonitrile

Ausbeute 68.0%

Lösungsmittel

methylene dichloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigedid not exceed -65° C
2. 2
   Waschenwashed twice with water
3. 3
   Trocknendried over sodium sulphate
4. 4
   Einengenconcentrated
5. 5
   Sonstigeto give a gum residue
6. 6
   SonstigeThe gum crystallized when it
7. 7
   Sonstigewas triturated with diethyl ether
8. 8
   FiltrationThe solid was collected by filtration
9. 9
   Sonstigerecrystallized from 2-propanol

Vorschrift

To a solution of 46.3 g (0.2 mole) of 4'-chloro-2-aminobenzophenone and 17.4 g (0.2 mole) of methylthioacetonitrile in 1 liter of methylene dichloride at a temperature of -70° C. was added dropwise 22.2 g (0.21 mole) of tert. butyloxychloride at a rate to ensure that the reaction temperature did not exceed -65° C. The resulting solution was allowed to warm to ambient temperature, washed twice with water, dried over sodium sulphate, and concentrated to give a gum residue. The gum crystallized when it was triturated with diethyl ether. The solid was collected by filtration and recrystallized from 2-propanol to yield 43.0 g (68%) of the title compound as a tan solid, m.p. 122° C.

Quelle