HRID1715350
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
To a stirred solution of D1 (1.0 eq) in THF (0.1 M) at RT was added a solution of LiOH (2.0 eq) in H2O (0.1 M) and the reaction mixture was stirred for 1 hr, then quenched by adding 6M HCl solution until pH=2. The organic solvent was evaporated and the product was extracted by DCM. Organic layers were washed with brine and dried (Na2SO4). Evaporation of the solvent under reduced pressure gave the crude product which was purified by flash column chromatography using Pentane to yield the desired compound as a brown oil. 1H NMR (300 MHz, CDCl3, 300K) δ 7.85-7.80 (1H, m), 7.32 (1H, d, J=4.2 Hz), 3.66 (1H, s).
WORKUP
后处理
- customquenched
- additionby adding 6M HCl solution until pH=2
- customThe organic solvent was evaporated
- extractionthe product was extracted by DCM
- washOrganic layers were washed with brine
- dry with materialdried (Na2SO4)
- customEvaporation of the solvent under reduced pressure
- customgave the crude product which
- customwas purified by flash column chromatography