HRID1429531

反应详情

EQUATION

反应方程式

HRID 1429531 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 tert-butyl 4-(6-bromobenzo[d]thiazol-2-yl)piperazine-1-carboxylate (300 mg, 0.753 mmol) in CH2Cl2 (6 mL) was added TFA (0.87 mL, 11.30 mmol). Upon completion of addition, the reaction mixture was stirred at rt for 3 hrs. After this time, the reaction mixture was diluted with CH2Cl2 and washed with aqueous NaOH (1 N, 5 mL) and brine (5 mL), and then dried (Na2SO4). The reaction mixture was filtered and then concentrated under reduced pressure to obtain Compound 13B as a light yellow solid (223 mg, 0.748 mmol, 99% yield). 1H NMR (500 MHz, chloroform-d) δ ppm 7.72 (s, 1H), 7.41 (s, 2H), 3.58-3.66 (m, 4H), 2.98-3.07 (m, 4H). LC/MS (m/z)=299 (M+H)+.

WORKUP

后处理

  1. additionUpon completion of addition
  2. washwashed with aqueous NaOH (1 N, 5 mL) and brine (5 mL)
  3. dry with materialdried (Na2SO4)
  4. filtrationThe reaction mixture was filtered
  5. concentrationconcentrated under reduced pressure