反应详情

温度

80 °C

2M Sodium hydroxide (1 ml, 2 mmol) was added to a solution of ethyl 4-[4-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indazol-1-yl]butanoate (D60) (N2666-13-A1) (0.062 g, 0.132 mmol) in ethanol (5 ml) and the reaction was heated to 80° C. to effect dissolution then left to cool for 2 hours. Evaporated, dissolved in ethyl acetate/water (25 ml of each) and acidified with acetic acid. Organic dried (magnesium sulphate), evaporated, azeotroped with 15 ml of toluene and triturated with ether. Filtered to give the title compound (42 mg) as a white solid. 5H (d6-DMSO, 400 MHz): 1.37 (6H, d), 2.09 (2H, m), 2.24 (2H, t), 4.54 (2H, t), 4.90 (1H, m), 7.47 (1H, d), 7.62 (1H, dd), 7.97 (1H, d), 8.01 (1H, d), 8.17 (1H, dd), 8.26 (1H, d), 8.56 (1H, s). MS (ES): C22H2135ClN4O4 requires 440; found (MH+) 441.

1. dissolutiondissolution
2. waitthen left
3. temperatureto cool for 2 hours
4. customEvaporated
5. dissolutiondissolved in ethyl acetate/water (25 ml of each) and
6. dry with materialOrganic dried (magnesium sulphate)
7. customevaporated
8. customazeotroped with 15 ml of toluene
9. customtriturated with ether
10. filtrationFiltered