反応 #54486

反応方程式

dihydrochloride

1-phenyl-2-(1-piperazinyl)-indole 3-carboxylic acid (4-methyl)-piperazide

2-(2-chloroethyl)-1,3-dioxolane

triethylamine

→

2-[4-(2-(1,3-dioxolan-2-yl)-ethyl)-1-piperazinyl]-1-phenyl indole 3-carboxylic acid (4-methyl)-piperazide

溶媒

chloroform

toluene

反応条件

後処理

1. 1
   温度was maintained at the boil for 40 hours
2. 2
   温度After cooling
3. 3
   洗浄washed three times with water
4. 4
   その他The resinous residue of the organic phase was chromatographed
5. 5
   洗浄The base was eluted as a resin
6. 6
   その他theoretical yield)

実験手順

A stirred mixture of 8 g (0.02 mol) of 1-phenyl-2-(1-piperazinyl)-indole 3-carboxylic acid (4-methyl)-piperazide, 9.45 g (0.07 mol) of 2-(2-chloroethyl)-1,3-dioxolane and 9.7 ml of triethylamine in 60 ml of toluene was maintained at the boil for 40 hours. After cooling, the mixture was diluted with 200 ml of chloroform, washed three times with water, and the solvent was eliminated in vacuo. The resinous residue of the organic phase was chromatographed using silica gel 60 (0.06-0.2 mm, deactivated by 10% of water, column size: 3 × 100 cm) with chloroform containing 10% methanol. The base was eluted as a resin. The yield amounted to 6.6 g (66% of the theoretical yield). The dihydrochloride melted at 215°-217° C.

出典