反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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) (1.5 g, 3.20 mmol) in hot ethanol (15 ml) was treated with sodium hydroxide (7.5 ml, 15.00 mmol) and stood for 1 hr. The solvents were evaporated and the residue partitioned between ethyl acetate/water. Acetic acid was added to adjust the pH to 5 and the layers separated. The organic layer was dried over magnesium sulphate and evaporated. The crude material was triturated with ether to give the title compound (1.1 g) as a white solid. 5H (d6-DMSO, 400 MHz): 1.37 (6H, d), 2.08 (2H, m), 2.23 (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.
WORKUP
后处理
- customThe solvents were evaporated
- customthe residue partitioned between ethyl acetate/water
- additionAcetic acid was added
- customthe layers separated
- dry with materialThe organic layer was dried over magnesium sulphate
- customevaporated
- customThe crude material was triturated with ether