반응 #1286192

반응 방정식

4'-chloro-2-aminobenzophenone

methylthioacetonitrile

tert. butyloxychloride

→

title compound

수율 68.0%

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

수율 68.0%

용매

methylene dichloride

반응 조건

후처리

1. 1
   기타did not exceed -65° C
2. 2
   세척washed twice with water
3. 3
   건조dried over sodium sulphate
4. 4
   농축concentrated
5. 5
   기타to give a gum residue
6. 6
   기타The gum crystallized when it
7. 7
   기타was triturated with diethyl ether
8. 8
   여과The solid was collected by filtration
9. 9
   기타recrystallized from 2-propanol

실험 절차

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.

출처