反応 #4452

ord-4003f3bd15224084afa096bd852af473

反応方程式

Clc1cc(-c2csc(Cc3ccccc3)n2)ccn1
2-benzyl-4-(2-chloro-4-pyridyl)thiazole
Cl.Cl.c1ccc(Cc2nc(-c3ccnc(N4CCCCC4)c3)cs2)cc1
2-benzyl-4-[2-(1-piperidyl)-4-pyridyl]thiazole dihydrochloride
収率 73.5%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to reflux for 16 hours
  2. 2
    濃縮The reaction mixture was concentrated
  3. 3
    ろ過filtered through celite
  4. 4
    洗浄the filtrate washed with water (2×)
  5. 5
    乾燥The ether layer was dried
  6. 6
    濃縮concentrated
  7. 7
    workup.ADDITIONtreated with an excess of dry hydrochloric acid

実験手順

A solution of 2-benzyl-4-(2-chloro-4-pyridyl)thiazole (1.00 g, 0.0035 mol) in piperidine (15 mL) was heated to reflux for 16 hours. The reaction mixture was concentrated, taken up in ether (50 mL), filtered through celite, and the filtrate washed with water (2×). The ether layer was dried and concentrated. The residue was taken up in ethanol (20 mL) and treated with an excess of dry hydrochloric acid. Careful dilution with ether afforded 2-benzyl-4-[2-(1-piperidyl)-4-pyridyl]thiazole dihydrochloride (525 mg, 49%). mp. 145° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04725606uspto-grants-1988_02