HRID968246

反应详情

EQUATION

反应方程式

HRID 968246 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 3-[(4-acetylpiperazin-1-yl)methyl]-5-methylphenylcarbamate (306 mg, 0.88 mmol) in CH2Cl2 (4 mL) was added TFA (4 mL) at room temperature. After 2 hours the mixture was concentrated. The residue was taken up in saturated NaHCO3 and extracted with CH2Cl2 (3×). The combined organic layers were dried (MgSO4), filtered, and concentrated to give 3-[(4-acetylpiperazin-1-yl)methyl]-5-methylaniline as a white solid. 1H-NMR (300 MHz, CDCl3) δ 6.52 (s, 1H), 6.48 (s, 1H), 6.43 (s, 1H), 3.62 (m, 4H), 3.45 (m, 2H), 3.39 (s, 2H), 2.40 (m, 4H), 2.25 (s, 3H), 2.08 (s, 3H).

WORKUP

后处理

  1. concentrationAfter 2 hours the mixture was concentrated
  2. extractionextracted with CH2Cl2 (3×)
  3. dry with materialThe combined organic layers were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated