反应详情

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.

1. customdid not exceed -65° C
2. washwashed twice with water
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated
5. customto give a gum residue
6. customThe gum crystallized when it
7. customwas triturated with diethyl ether
8. filtrationThe solid was collected by filtration
9. customrecrystallized from 2-propanol