HRID2295793

反应详情

EQUATION

反应方程式

HRID 2295793 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 1 L rocking Parr hydrogenator was charged with a solution containing 19.11 g of 4-(4-chloro-5,6,7,8-tetrahydro-1-naphthoxy)-3,5-dimethyl-1-nitrobenzene in 600 mL of toluene. To this was then added 1.0 g of 5% platinum on carbon. This was then placed under an atmosphere of hydrogen at 100 psi. The internal pressure was maintained between 80 and 100 psi while hydrogen uptake continued. When the hydrogen uptake ceased, the contents of the hydrogenator were removed and the vessel washed with toluene. The washings were combined with the reaction mixture. This was then filtered through celite. Removal of the solvents afforded 17.30 g of pale yellow solid. mp 126°-135° C. NMR(CDCl3): δ1.6-1.8 (m, 4H), 2.0 (S, 6H), 2.6-2.9 (m, 4H), 3.45 (S, 2H), 6.13 (d, J=9 Hz, 1H), 6.37 (S, 2H), 6.93 (d, J= 9 Hz, 1H).

WORKUP

后处理

  1. additionwas charged with a solution
  2. customthe contents of the hydrogenator were removed
  3. washthe vessel washed with toluene
  4. filtrationThis was then filtered through celite
  5. customRemoval of the solvents