HRID2189814

反应详情

EQUATION

反应方程式

HRID 2189814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvents were evaporated
  2. customthe residue partitioned between ethyl acetate/water
  3. additionAcetic acid was added
  4. customthe layers separated
  5. dry with materialThe organic layer was dried over magnesium sulphate
  6. customevaporated
  7. customThe crude material was triturated with ether