HRID1811585

反应详情

EQUATION

反应方程式

HRID 1811585 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 2,4-dimethylpyridin-3-amine (2.0 g, 16 mmol) in CH2Cl2 (20 mL), was added a solution of bromine (3.16 g; 20 mmol) in CH2Cl2 (5 mL) at 0° C. for 5 min. The reaction was concentrated under vacuum. The reaction was poured into H2O (50 mL), extracted with CH2Cl2, washed with Na2SO3 solution, and dried over MgSO4. The CH2Cl2 was concentrated under vacuum to afford the crude compound. The crude was purified over SiO2 to afford to give 6-bromo-2,4-dimethylpyridin-3-amine. 1HNMR (CDCl3, 400 MHz) δ 2.10 (s, 3H), 2.31 (s, 3H), 4.85-5.10 (b, 2H), 7.05 (s, 1H). Exact mass calculated for C7H9BrN2 201.06. found 202.3 (MH+).

WORKUP

后处理

  1. concentrationThe reaction was concentrated under vacuum
  2. additionThe reaction was poured into H2O (50 mL)
  3. extractionextracted with CH2Cl2
  4. washwashed with Na2SO3 solution
  5. dry with materialdried over MgSO4
  6. concentrationThe CH2Cl2 was concentrated under vacuum
  7. customto afford the crude compound
  8. customThe crude was purified over SiO2
  9. customto afford