関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetate | HCID 175 | — |
| 反応物 | Nitrate | HCID 943 | — |
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfate Ion | HCID 1117 | — |
| 反応物 | Cyproheptadine | HCID 2913 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 6-Methyl-2,4,6-trinitro-2,4,6-triazahexanol | HCID 57262353 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Acetoxy-2,4,6-trinitro-2,4,6-triazaheptane | HCID 19797990 | — |
反応手順
"Acetate or nitrate of 6-alkyl-2,4,6-trinitro-2,4,6-triazahexanol. Jiri Denkstein and Vladimir Kaderabek. Czech. 98,248, Jan. 15, 1961, Appl. Nov. 13, 1959. The described method is the nitrolysis of N-alkylhexamethylene-tetraminium nitrate, sulfate, or acetate with a mixt. of HNO3 with Ac2O, or anhydride of HNO3. Thus, a mixt. of 30 g N-methylhexamethylenetetraminium nitrate (I) and 49 ml. AcOH added during 15-30 min with stirring at 15°-20° to the mixt. of 52 ml. 98-9% HNO3, and 48 ml. Ac2O under stirring, the temp. increased to 75° and kept 15 min. gave after cooling to 20°-5° 22.2 g cryst. 6-methyl-2,4,6-trinitro-2,4,6-triazahexanol (II). The reactin mixt. dild. with water gave addnl. 5.3 g II. The total yield was 27.5 g of a product, m. 151°-3° , i.e., 68% of theory calcd. on I."
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05243075 |
|---|
| 出典データセット | uspto-grants-1993_09 |
|---|
| ORD ID | ord-441df664c30c4a9e9bf4d09ba8dd20c5 |
|---|
| 出典メモ | uspto-grants-1993_09 |
|---|