Synthesizing method of deuterated octogen
A technology of octogen and synthesis method, which is applied in the field of preparation of organic compounds and can solve problems such as synthesis that has not yet been reported.
Image
Examples
Embodiment 1
[0069] A kind of synthetic method of deuterated Octogen, the steps are as follows:
[0070] 1) Put 1.0g of deuterated paraformaldehyde in a 25mL two-neck round bottom flask, add 2.0mL of deionized water, add 3.0mL of ammonia water, and control the temperature at 15-50°C during the addition. After the feeding is completed, the temperature of the oil bath is controlled at 15-50°C to react for 68 hours. After the reaction is completed, part of the tert-butanol solution is added to the reaction solution. 95%.
[0071] 2) Put 0.4g of the synthesized deuterated urotropine in a 25mL two-necked round-bottomed flask, add 0.2g of ammonium acetate, and dropwise add 0.8g of acetic anhydride. The reaction was carried out for 1 h at room temperature, and then the reaction was continued for 1 h at room temperature. Heat in an oil bath and keep the system temperature at 25-35°C for 40 hours. Cool to get DAPT-d 10 The reaction solution can be directly used in the next reaction without puri...
Embodiment 2
[0075] A kind of synthetic method of deuterated Octogen, the steps are as follows:
[0076] a. Dissolve deuterated formaldehyde substances in the solvent at 0°C, add ammonia compounds, keep the reaction temperature at 0°C, and react for 100 hours. After the reaction is completed, the solvent is distilled off, and the residue is the prepared deuterated urethane Tropin (referred to as HMTA-d 12 );
[0077] The deuterated formaldehyde substance can be a 5% deuterated formaldehyde aqueous solution or deuterated paraformaldehyde;
[0078] The solvent may be one or a mixture of two or more of water, alcohol, halogenated hydrocarbon, ether, amide, sulfoxide, and hydrocarbon compounds;
[0079] The ammonia compound can be ammonium salt, ammonia gas, ammonia water, liquid ammonia or an organic solution of ammonia gas;
[0080] Convert deuterated formaldehyde substances into deuterated formaldehyde measurement, the molar amount of deuterated formaldehyde and NH 3 The ratio of the mo...
Embodiment 3
[0094] A kind of synthetic method of deuterated Octogen, the steps are as follows:
[0095] a. Dissolve deuterated formaldehyde substances in the solvent at 70°C, add ammonia compounds, keep the reaction temperature at 70°C, and react for 1h. After the reaction is completed, the solvent is distilled off, and the residue is the prepared deuterated urethane Tropin (referred to as HMTA-d 12 );
[0096] The deuterated formaldehyde substance can be deuterated formaldehyde aqueous solution or deuterated paraformaldehyde with a mass percentage content of 60%;
[0097] The solvent may be one or a mixture of two or more of water, alcohol, halogenated hydrocarbon, ether, amide, sulfoxide, and hydrocarbon compounds;
[0098] The ammonia compound can be ammonium salt, ammonia gas, ammonia water, liquid ammonia or an organic solution of ammonia gas;
[0099] Convert deuterated formaldehyde substances into deuterated formaldehyde measurement, the molar amount of deuterated formaldehyde a...
PUM
Login to View More Abstract
Description
Claims
Application Information
- IPC
- C07D257/02
- CPC
- C07D257/02; C07B2200/05
- Inventors
- 杨海君; 白亮飞