Chloroacetonitrile → HCID 57754432, compound

Participants

Reaction Steps

A mixture of 0.3 g (0.74 mmol) of the product from Example 1, step 6 and 0.3 g (0.74 mmol) of Lawesson's reagent (2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide) in 30 ml of toluene is refluxed for 15′. The solution is washed with water, dried and concentrated. The residue is dissolved in 25 ml of dichloromethane and 0.07 g (0.93 mmol) of chloroacetonitrile and 0.14 ml (0.10 g; 1.0 mmol) of N,N,N-triethylamine are added. The whole is stirred overnight at room temperature. The solution is washed with water, dried, concentrated and chromatographied trough SiO2 eluting with dichloromethane/methanol 98:2. The yield of title product is 0.12 g (35%).

Provenance & Evidence