反応 #63461

反応方程式

6-(3,4-Dihydro-1,4(2H)-benzoxazin-6-yl)-2,3,4,5-tetrahydropyridazin-3-one

triethylamine

3,4-dimethoxybenzoylchloride

→

6-(3,4-Dihydro-4-(3,4-dimethoxyphenylcarbonyl)-1,4(2H)-benzoxazin-6-yl)-2,3,4,5-tetrahydropyridazin-3-one

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度the mixture heated
2. 2
   温度at reflux for four hours
3. 3
   洗浄The solution was washed with sodium bicarbonate solution
4. 4
   その他evaporated to dryness
5. 5
   その他The residue was chromatographed on silica gel eluting with 1:1 ethyl acetate
6. 6
   その他The title compound was collected as white needles, mp 207°-208° C.

実験手順

6-(3,4-Dihydro-1,4(2H)-benzoxazin-6-yl)-2,3,4,5-tetrahydropyridazin-3-one was dissolved in methylene chloride and 1.1 equivalent of triethylamine. 1.1 equivalent of 3,4-dimethoxybenzoylchloride was added and the mixture heated at reflux for four hours. The solution was washed with sodium bicarbonate solution and then evaporated to dryness. The residue was chromatographed on silica gel eluting with 1:1 ethyl acetate:ethyl ether. The title compound was collected as white needles, mp 207°-208° C.

出典