HRID467040

反应详情

EQUATION

反应方程式

HRID 467040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Aminomethyl-1-hydroxy-1,2,3,4-tetrahydronaphthalene, the product of Example 7, was refluxed in a 2N solution of hydrogen chloride in 2-propanol (250 mL) for 5 hours. A portion of the 2-propanol was removed under reduced pressure to give a slurry. Diethyl ether was added to precipitate the hydrochloride salt. The resulting suspension was then filtered. The filter cake was then recrystallized from methanol/diethyl ether to give 16.18 g (59% yield based on 1,2,3,4-tetrahydronaphthalene-1-one) of the desired product as a light tan solid; 1H NMR (CD3OD) δ 2.31-2.40 (m, 2H), 2.80 (t, 2H, J=8 Hz), 4.0 (s, 2H), 6.26 (t, 1H, J=4.5 Hz), 7.19-7.29 (m, 4H).

WORKUP

后处理

  1. customA portion of the 2-propanol was removed under reduced pressure
  2. customto give a slurry
  3. customto precipitate the hydrochloride salt
  4. filtrationThe resulting suspension was then filtered
  5. customThe filter cake was then recrystallized from methanol/diethyl ether