[C:1]([Cl:4])([Cl:3])=O.[CH2:5]1[C@H:17]2[N:8]([CH2:9][C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:15]=3[CH2:16]2)C(=S)[S:6]1>C1(C)C=CC=CC=1.O1CCCC1>[Cl-:3].[Cl:4][C:1]1[S:6][CH2:5][C@@H:17]2[CH2:16][C:15]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[CH2:9][N+:8]=12A solution (20 cc.) containing 2 mols per liter of phosgene in toluene, is added dropwise, in the absence of moisture, whilst stirring and at a temperature of about 20° C ., to a solution of (S)-1,5,10,10a-tetrahydrothiazolo[3,4-b]isoquinoline-3-thione (2.2 g.) in tetrahydrofuran (25 cc.). The mixture becomes cloudy after 15 minutes; it is stirred for 5 hours and then heated to 50° C. for 1 hour. The solvents are evaporated under reduced pressure (25 mm. Hg ) at 60° C. to give (S)-3-chloro-1,5,10,10a-tetrahydrothiazolo[3,4-b]isoquinolinium chloride (2.6 g.) in the form of a very hygroscopic white crystalline powder.
読み込み中…
