HRID1715350

反应详情

EQUATION

反应方程式

HRID 1715350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customquenched
  2. additionby adding 6M HCl solution until pH=2
  3. customThe organic solvent was evaporated
  4. extractionthe product was extracted by DCM
  5. washOrganic layers were washed with brine
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of the solvent under reduced pressure
  8. customgave the crude product which
  9. customwas purified by flash column chromatography