反応 #156189

反応方程式

Triphenyl phosphine

di-tert-butyl azodicarboxylate

6-hydroxy-2H-isoquinolin-1-one

3-[(2-pyridin-3-ylethyl)pyridin-4-ylmethylamino]propan-1-ol

hydrogen chloride ethyl acetate

→

title compound

6-{3-[(2-pyridin-3-ylethyl)pyridin-4-ylmethylamino]propoxy}-2H-isoquinolin-1-one trihydrochloride

溶媒

tetrahydrofuran

ethyl acetate

反応条件

後処理

1. 1
   その他condensed under reduced pressure
2. 2
   その他the residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=1:0→4:1)
3. 3
   その他condensed under reduced pressure
4. 4
   workup.STIRRINGwas stirred at room temperature for 30 minutes
5. 5
   その他The generated insoluble matter was separated by filtration
6. 6
   その他was dried

実験手順

Triphenyl phosphine (51 mg) and di-tert-butyl azodicarboxylate (45 mg) were added to a tetrahydrofuran (THF) solution (1.5 ml) of 6-hydroxy-2H-isoquinolin-1-one (29 mg), and 3-[(2-pyridin-3-ylethyl)pyridin-4-ylmethylamino]propan-1-ol (40 mg). The mixture was stirred overnight. After the reaction mixture was condensed under reduced pressure, the residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=1:0→4:1). The purified product was condensed under reduced pressure. A 4N-hydrogen chloride ethyl acetate solution (0.06 ml) was added to an ethyl acetate solution of the residue, which was stirred at room temperature for 30 minutes. The generated insoluble matter was separated by filtration, and was dried to produce the title compound (31.4 mg) as a white powder.

出典