HRID1909782
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 the product of step 3 (90 mg, 0.21 mmol) in dioxane (2 ml) was added 4M HCl in dioxane (0.5 ml, 2.1 mmol), and stirred at room temperature for 4 h. After the solvent was removed, the crude material was triturated with ether to afford the title product (60 mg, 83%); 1HNMR (400 MHz, CD3OD) δ 7.90 (d, J=8.4 Hz, 2H), 7.82 (d, J=3.2 Hz, 1H), 7.55 (d, J=3.6 Hz, 1H), 7.07 (s, 4H), 7.00 (d, J=8.8 Hz, 2H), 4.22 (dd, J=10.4, 3.2, 1H), 4.14 (m, 1H), 4.04 (m, 1H), 3.38 (m, 2H), 2.28 (m, 1H), 2.14 (m, 2H), 1.92 (m, 1H); LC/MS (ESI+) 88%; m/z: 353 (M+1, 100).
WORKUP
后处理
- customAfter the solvent was removed
- customthe crude material was triturated with ether