HRID1839910
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 1.2 M solution of lithium hydroxide (300 μL, 0.36 mmol) was added to a solution of [4-(4-benzyloxycarbonylmethoxy-3,5-diiodo-benzoyl)-2,6-diiodo-phenoxy]-acetic acid benzyl ester (prepared according to Example 12, 76 mg, 0.075 mmol) in 2.4 mL THF. The suspension was stirred for 48 hours, after which time the mixture was poured into 1 M HCl. The resulting white precipitate was isolated by filtration, rinsed with water, and dried in vacuo, yielding the title compound as a white powder (52 mg, 83%). 1H NMR (400 MHz, DMSO-d6): δ 13.17 (br. s, 2H), 8.09 (s, 4H), 4.55 (s, 4H). HPLC (40-90), 10.29 min. LRMS (EI−) calc'd for [C17H10I4O7—H] 832.7, found 832.6.
WORKUP
后处理
- customThe resulting white precipitate was isolated by filtration
- washrinsed with water
- customdried in vacuo