Sodium methanethiolate → HCID 178503807, compound

Participants

Reaction Steps

To a suspension of sodium thiomethoxide (230 mg, 3.2 mM) in dimethylformamide (20 mL), was added in one portion 2-(2-bromoethyl)-7-chloro-4-hydroxy-1,2,5,10-tetrahydropyridazino-[4,5-b]quinoline-1,10-dione (0.4 g, 1.08 mM, prepared in Example 4a. of docket No. 37811) as a dry powder. This mixture was warmed to gentle reflux for aboutthree hours. At this point the heat was removed and the reaction mixture was poured into ice cold 1.2N HCl (l00 mL) and stirred about one hour. Theresulting precipitate was vacuum filtered and washed with water and ether, then vacuum dried at 50° C. to yield 330 mg (91%) of the title compound as an off white powder. mp=275°-277° C.; MS: 338(M+1).

Provenance & Evidence