反応 #655111

反応方程式

pentaerythrityl tetranitrate

hydrazine hydrate

→

Pentaerythrityl trinitrate

溶媒

dioxane

ethanol

反応条件

後処理

1. 1
   workup.ADDITIONare added in portions over 1 hour
2. 2
   温度The reaction mixture is then refluxed for a further 2.5 hours
3. 3
   その他The solvents are evaporated off at 15 mm Hg
4. 4
   抽出the residue is extracted
5. 5
   抽出no longer decreases on extraction
6. 6
   その他The aqueous extracts (A) are collected
7. 7
   workup.DISSOLUTIONthe residual oily layer is dissolved in twice its volume of ethanol
8. 8
   その他Any white precipitate of PETN which has separated out
9. 9
   ろ過is filtered off after 24 hours
10. 10
    その他Ethanol is evaporated off from the filtrate at 15 mm Hg

実験手順

158 g (0.5 mol) of pentaerythrityl tetranitrate (PETN) are dissolved in a boiling mixture of 300 ml of dioxane and 300 ml of ethanol, and different amounts of aqueous hydrazine hydrate solution (1.5-4 mol) are added in portions over 1 hour. The reaction mixture is then refluxed for a further 2.5 hours. The solvents are evaporated off at 15 mm Hg and the residue is extracted by shaking several times with 100 ml portions of water, as required, until the volume of the oil layer no longer decreases on extraction. The aqueous extracts (A) are collected and the residual oily layer is dissolved in twice its volume of ethanol. Any white precipitate of PETN which has separated out is filtered off after 24 hours; m.p.=132° C., nitrogen content: 17.35%; m.p.=141° C. (2×acetone); nitrogen content: conforms. Ethanol is evaporated off from the filtrate at 15 mm Hg. The viscous oily residue consists of crude pentaerythrityl trinitrate (PETriN); nitrogen content: conforms.

出典