HRID1245057

反应详情

EQUATION

反应方程式

HRID 1245057 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-bromophthalic acid (3.0 g, 12.24 mmol) in 30 mL of THF was added a solution of borane-THF complex (1.0M) dropwise at 0° C. The solution was warmed to rt and stirred for 3 h. The reaction mixture was quenched by addition of HCl (2N) at 0° C. The product was extracted with ethyl acetate and washed with sat. NaCl, dried over Na2SO4, and concentrated under reduced pressure to afford 2.8 g (100%) of 4-bromo-2-hydroxymethylbenzyl alcohol as a colorless oil. 1H NMR (CDCl3) 7.28 (m, 2H), 7.26 (m, 1H), 4.69 (s, 4H), 2.80 (bs, 2H).

WORKUP

后处理

  1. customThe reaction mixture was quenched by addition of HCl (2N) at 0° C
  2. extractionThe product was extracted with ethyl acetate
  3. washwashed with sat. NaCl
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under reduced pressure