Water → Cloturin

Participants

Reaction Conditions

Reaction Steps

A suspension of 6-mercaptopurine monohydrate (17.0 g, 0.1 mole) in dimethylformamide (150 ml) is treated with triethylamine (10.1 g, 0.1 mole) and the solid is dissolved by warming of the mixture to 50°-60° C. The solution is cooled to 15° C. and 2-chloroethylisocyanate (11.6 g, 0.11 mole) is dripped in under cooling with tap water to 15°-20° C. The reaction mixture is stirred at this temperature for 2 hours, and the precipitated product is collected on filter, washed with acetone and dried under reduced pressure at a temperature of approx. 50° C. to give 20.7 g (80%) of the title compound Ia, melting at 221°-223° C. UV absorption spectrum (in dimethylsulfoxide), λ max 326 nm (log ε4.33).

Provenance & Evidence