反应 #4302

反应方程式

2-chloroethyl phenyl sulfide

potassium iodide

isopropylamine

→

white crystalline solid

收率 76.9%

N-[2-(Phenylthio)ethyl]-2-propanamine hydrochloride

收率 76.9%

反应条件

后处理

1. 1
   其他The solvent was removed in vacuo
2. 2
   其他the residue was partitioned between methylene chloride and dilute sodium hydroxide
3. 3
   萃取The methylene chloride solution was extracted with dilute sulfuric acid
4. 4
   萃取The acidic extract
5. 5
   萃取the basic solution was extracted with methylene chloride
6. 6
   干燥The methylene chloride solution was dried over magnesium sulfate
7. 7
   其他the solvent was removed in vacuo
8. 8
   其他to give an oil
9. 9
   其他the salt was recrystallized from methanol-ether

实验过程

A solution of 25 g (0.145 mole) of 2-chloroethyl phenyl sulfide and 1 g (0.006 mole) of potassium iodide in 500 ml of isopropylamine was heated in a bomb at 120° C. for 24 hr. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was extracted with dilute sulfuric acid. The acidic extract was made basic with 50% sodium hydroxide, and the basic solution was extracted with methylene chloride. The methylene chloride solution was dried over magnesium sulfate and the solvent was removed in vacuo to give an oil. This was converted to the hydrochloride salt, and the salt was recrystallized from methanol-ether to give 25.77 g (76.9%) of white crystalline solid, m.p. 124.5°-125.5° C.

来源