β型氘代奥克托今(β-HMX-d_8)的合成

Synthesis of β-Phase Deuterated Octogen(β-HMX-d_8)

为了制备高纯度和高氘代率的氘代奥克托今(HMX-d_8),在以非氘代多聚甲醛为原料合成HMX的工艺基础上,以氘代多聚甲醛为原料,成功实现了氘代奥克托今(β-HMX-d_8)的合成,总产率达58.5%。以丙酮为晶型转化溶剂,采用重结晶的方法得到β-HMX-d_8。采用紫外可见光谱(UV-vis)、傅里叶变换红外光谱(FT-IR)、核磁共振氢谱(1 H NMR)、核磁共振碳谱(13 C NMR)、热重-微分热重(TG-DTG)、差示扫描量热(DSC)和X射线粉末衍射(XRD)等对中间体和目标产物进行了分析表征。以马来酸酐为内标,采用核磁法,测得所合成β-HMX-d_8的氘代率为99.75%。采用面积归一法,HPLC测定所合成β-HMX-d_8的纯度为99.27%。

Based on the preparation technology of non-deuterated HMX using paraformaldehyde as raw material,deuterated octagon（β-HMX-d8）was successfully synthesized with a total yield of 58.5% from deuterated paraformaldehyde.The β-HMX-d8 was obtained via recrystallization method using acetone as the crystal transformation solvent.The intermediates and final products were characterized by ultraviolet-visible spectroscopy（UV-Vis）,Fourier transform infrared（FT-IR）spectroscopy,1 H-nuclear magnetic resonance（~1 H NMR）spectroscopy,^（13） C-nuclear magnetic resonance（^（13） C NMR）spectroscopy,thermogravimetry-derivative thermogravimetry（TGDTG）,differential scanning calorimetry（DSC）,or x-ray powder diffraction（XRD）.The deuterated ratio of systhesized β-HMX-d8 is 99.75% measured by NMR method with maleic anhydride as an internal standard.The purity of HMX-d8 is 99.27% determined by HPLC via area normalization method.