反応 #521352

ord-12931a982b2c46bda5dc1e14be940140

反応方程式

CO
methanol
Cl
hydrochloride
COC(C)=O
methyl acetate
Cl
hydrogen chloride
N#CC(NCCc1cccs1)c1ccccc1Cl
[2-(2-thienyl)ethylamino](2-chorophenyl)acetonitrile
Cl.NC(=O)C(NCCc1cccs1)c1ccccc1Cl
[2-(2-Thienyl)ethylamino](2-chlorophenyl)acetamide Hydrochloride

反応条件

温度
22.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他prepared
  2. 2
    その他gradually the hydrochloride of the resulting “acid amide” precipitates, in the form of white crystals
  3. 3
    ろ過The crystals are collected by filtration
  4. 4
    洗浄washed with methyl acetate
  5. 5
    その他dried

実験手順

Into 1200 ml of methyl acetate 204 g (5.6 mol) of hydrogen chloride gas is introduced at 15-25° C., and to the solution are added 221.4 g (0.8 mol) of the [2-(2-thienyl)ethylamino](2-chorophenyl)acetonitrile, prepared as described in Example 1., and 48 ml (1.2 mol) of methanol. The mixture is stirred at 20-25° C. for 6 hours. In the course of the reaction first the hydrochloride of the starting “nitrile”, then gradually the hydrochloride of the resulting “acid amide” precipitates, in the form of white crystals. The crystals are collected by filtration, washed with methyl acetate and dried. Weight: 249 g (94%) mp.: 231-232° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06670486B1uspto-grants-2003_12