反応 #4300

反応方程式

ether

2-chloroethylphenylsulfone

phenethylamine

triethylamine

→

white crystalline solid

収率 89.1%

N-[2-(Phenylsulfonyl)ethyl]benzeneethanamine, hydrochloride hemihydrate

収率 89.1%

溶媒

methanol

hydrogen chloride

acetonitrile

反応条件

後処理

1. 1
   その他The solvent was removed in vacuo
2. 2
   その他the residue was partitioned between methylene chloride and dilute sodium hydroxide
3. 3
   乾燥The methylene chloride solution was dried over magnesium sulfate
4. 4
   その他the solvent was removed in vacuo
5. 5
   その他to give an oil
6. 6
   workup.ADDITIONwas added
7. 7
   その他A white solid precipitated

実験手順

A mixture of 70.23 g (0.344 mole) of 2-chloroethylphenylsulfone, 41.92 g (0.343 mole) of phenethylamine and 60 ml of triethylamine in 800 ml of acetonitrile was stirred at room temperature for 18 hr. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol and excess of ethereal hydrogen chloride was added and ether was added. A white solid precipitated to give 68.39 g (60%) of white crystalline solid, m.p. 194°-196° C.

出典