反应详情

温度

20 °C

(S)-3-Methylthio-1,5,10,10a-tetrahydrothiazolo[3,4-b]isoquinolinium iodide (7.2 g) is added to a solution of 5-amino-3-ethoxymethylisoquinoline (4.1 g) in pyridine (150 cc). The suspension is stirred for 24 hours at a temperature of about 20° C. The insoluble material gradually dissolves. The solution is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at 60° C. The residue is dissolved in a mixture of methylene chloride (100 cc) and N sodium hydroxide solution (100 cc). The organic phase is decanted, washed with water (50 cc), dried over magnesium sulphate and filtered and the filtrate is evaporated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa). The residue is recrystallised from isopropyl alcohol (80 cc). (S)-3-[(3-Ethoxymethylisoquinol-5-yl)imino]-1,5,10,10a-tetrahydrothiazolo[3,4-b]isoquinoline (5.2 g) is thus obtained in the form of a pale yellow solid melting at 88° C.

1. dissolutionThe insoluble material gradually dissolves
2. concentrationThe solution is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at 60° C
3. dissolutionThe residue is dissolved in a mixture of methylene chloride (100 cc) and N sodium hydroxide solution (100 cc)
4. customThe organic phase is decanted
5. washwashed with water (50 cc)
6. dry with materialdried over magnesium sulphate
7. filtrationfiltered
8. customthe filtrate is evaporated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa)
9. customThe residue is recrystallised from isopropyl alcohol (80 cc)