HRID11428

反应详情

EQUATION

反应方程式

HRID 11428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Bromophenylethylamine hydrochloride (9.44 g) was added to THF (60 ml) containing triethylamine (12.24 ml) and stirred-under argon at 5° C. during the portionwise addition over 15 minutes of 4-methylphenylsulphonyl chloride (11.44 g). The slurry was diluted with THF (50 ml) and stirred for 16 h. The solid was filtered off, washed with THF and the filtrate evaporated. The residue was dissolved in ethyl acetate, washed with 1N hydrochloric acid, water, brine and dried (MgSO4). Chromatography on flash silica, eluting with 0 to 25% ethyl acetate in isohexane gave the product (9.67 g).

WORKUP

后处理

  1. filtrationThe solid was filtered off
  2. washwashed with THF
  3. customthe filtrate evaporated
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with 1N hydrochloric acid, water, brine
  6. dry with materialdried (MgSO4)
  7. washChromatography on flash silica, eluting with 0 to 25% ethyl acetate in isohexane