ENDOXABAN
2-amino-5-methyl-4,5,6,7-tetrahydro thiazolone [5,4-c] pyridine
(Reference Example 1) 2-amino-5-methyl-4,5,6,7-tetrahydro thiazolone [5,4-c] pyridine (1-n) (The method described in WO 2005/047296 Pamphlet )
[0091]
[Of 35] in 2-PrOH (1.44L) solution was heated to 50 ℃ 1- methyl-4-piperidone (180.0g), 2-PrOH (360mL) solution of cyanamide (67.0g), and sulfur powder (51.0 g) it was added. Pyrrolidine (13.3mL) was added to the reaction mixture, after stirring for 2 hours at 50 ℃, followed by stirring overnight and allowed to cool to room temperature. The reaction mixture was cooled to 10 ℃ less in an ice water bath and stirred for 1 hour at the same temperature. Is filtered and the precipitated crystals were washed with 2-PrOH (540mL), the title compound was dried under reduced pressure at 40 ℃ (209.9g, 78%) was obtained.
[0092]
1 H-NMR (CDCl 3 ) ppm: 4.86 (Br, 2H), 3.47-3.46 (t, 2H, J = 1.9 Hz), 2.78-2.71 (M, 2H), 2.71-2.65 (M, 2H), 2.47 . (s, 3H)
MS (FAB) M / z: 170 (M + H) +
elemental analysis: C 7 H 11 N 3 as S,
theoretical value: C, 49.68; H, 6.55; N, 24.83; S, 18.95
measured value: C, 49.70; H, 6.39; N, 24.91; S, 19.00.
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MS (FAB) M / z: 170 (M + H) +
elemental analysis: C 7 H 11 N 3 as S,
theoretical value: C, 49.68; H, 6.55; N, 24.83; S, 18.95
measured value: C, 49.70; H, 6.39; N, 24.91; S, 19.00.
DRUG APPROVALS BY DR ANTHONY MELVIN CRASTO .....FOR BLOG HOME CLICK HERE
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