関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Isopropylamine | HCID 6363 | — |
| 反応物 | Sodium dicyanamide | HCID 4350929 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | HCID 178457589 | HCID 178457589 | 97.2% |
反応手順
All the above-named compounds except N-[1-(9,10 dihydro-9,10 dioxo)anthracenyl]-N'-(1-methylethyl)imido dicarbonimidic diamide hydrochloride are commercially available. N-[1-(9,10 dihydro-9,10 dioxo)anthracenyl]-N'-(1-methylethyl)imido dicarbonimidic diamide hydrochloride, however, is a novel compound and was synthesized as follows: A three liter round bottomed flask was charged with 18.2 g (3.09 mole) of isopropyl amine. After cooling the flask to -70° C. in a dry ice and acetone bath, 304.5 g of concentrated (37%) hydrochloric acid (3.09 mole) was added. The mixture was warmed to room temperature and water was removed with a rotary evaporator at aspirator pressure. To the dry residue was added 275.3 g (3.09 mole) of sodium dicyanamide and 760 ml of 1-butanol. The mixture was heated under reflux for three hours and then the butanol was removed with a rotary evaporator at aspirator pressure. To the residue in the flask was added 1800 ml of 1,4-dioxane. A slightly sticky precipitate was formed which was filtered and recrystallized from four liters of 1,4-dioxane to yield 379 g of N-cyano-N'-isopropylguanidine as a co-precipitate with some NaCl, 1,4-dioxane, and isopropylamine. Calc. for C5H10N4 (NaCl)0.1(C4H8O2)0.1(C3H9N)0.15 Calc: C 46.94; H 8.18; N 38.83; C12.37 Found: C 46.85; H 8.27; N 38.42; Cl 2.44
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05385842 |
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| 出典データセット | uspto-grants-1995_01 |
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| ORD ID | ord-5c368781f5a84581a7942093343179d8 |
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| 出典メモ | uspto-grants-1995_01 |
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