反応 #1005939

反応方程式

1-(4-chlorophenyl)-3-[(Z)-3-iodobut-2-enoxy]pyrazole

N-methylcarbamic acid methyl ester

potassium phosphate

N,N′-dimethylethylene diamine

→

Methyl N—[(Z)-3-[1-(4-chlorophenyl)pyrazol-3-yl]oxy-1-methyl-prop-1-enyl]-N-methyl-carbamate

溶媒

toluene

反応条件

後処理

1. 1
   その他After removal of the solvents in vacuo the crude product
2. 2
   その他has been purified by chromatography on 50 g silica with MTBE/hexane (1:3)

実験手順

1.50 g (4.00 mmol) 1-(4-chlorophenyl)-3-[(Z)-3-iodobut-2-enoxy]pyrazole, 0.43 g (4.81 mmol) N-methylcarbamic acid methyl ester (9), 76 mg (0.4 mmol) copperiodide, 1.27 g (6.00 mmol) potassium phosphate and 71 mg (0.80 mmol) N,N′-dimethylethylene diamine in 14 ml toluene have been stirred for 1.5 d at 100° C. After removal of the solvents in vacuo the crude product has been purified by chromatography on 50 g silica with MTBE/hexane (1:3). Yield 0.67 g. 1H-NMR (CDCl3): δ=1.90 (s); 3.05 (s); 3.70 (s); 4.68 (m); 5.63 (m); 5.90 (d); 7.35 (m); 7.55 (m); 7.68 (d).

出典