반응 #655111

반응 방정식

pentaerythrityl tetranitrate

hydrazine hydrate

→

Pentaerythrityl trinitrate

용매

dioxane

ethanol

반응 조건

후처리

1. 1
   workup.ADDITIONare added in portions over 1 hour
2. 2
   온도The reaction mixture is then refluxed for a further 2.5 hours
3. 3
   기타The solvents are evaporated off at 15 mm Hg
4. 4
   추출the residue is extracted
5. 5
   추출no longer decreases on extraction
6. 6
   기타The aqueous extracts (A) are collected
7. 7
   workup.DISSOLUTIONthe residual oily layer is dissolved in twice its volume of ethanol
8. 8
   기타Any white precipitate of PETN which has separated out
9. 9
   여과is filtered off after 24 hours
10. 10
    기타Ethanol is evaporated off from the filtrate at 15 mm Hg

실험 절차

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.

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