関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 2,4,6-Trinitrotoluene | HCID 8376 | — |
| 反応物 | 2-Chloro-1,3,5-trinitro-4-[2-(2,4,6-trinitrophenyl)ethenyl]benzene | HCID 329469 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(2,4,6-Trinitrobenzyl)-2,2',4,4',6,6'-hexanitrostilbene | HCID 54495584 | — |
反応手順
The reaction of 4.5 g (0.02 mole) of TNT with 4.6 g (0.01 mole) of 3-chloro-2,2',4,4',6,6'-hexanitrostilbene was carried out as in the above reactions. The crude reaction product, after extraction with methanol was a brittle mass which was dissolved in 50 mol of acetonitrile, diluted with an equal volume of methanol and heated on a hot plate with magnetic stirring. Light yellow crystals separated and were filtered off, washed well with methanol and dried. This material weighed 4.8 g, 71% of the theoretical yield, melted at 168°-170° (dec), and elemental analysis showed that it contained a mole of acetonitrile. Calcd for C23H12N10O18 : N, 19.6. Found: N, 19.7, 19.4. Recrystallized from 50 ml of THF with 50 ml of methanol added to the hot THF solution after filtering, the product separated in very fine, almost colorless crystals, mp 210°-211°C. Anal. Calcd for C21H9N9O18 : C, 37.2; H, 1.3; N, 18.8. Found: C, 37.5, 37.7; H, 1.6, 1.5; N, 19.0, 18.4.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03941853 |
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| 出典データセット | uspto-grants-1976_03 |
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| ORD ID | ord-2af45799271042048a33356e61663dfe |
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| 出典メモ | uspto-grants-1976_03 |
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