関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydroxylamine | HCID 787 | — |
| 反応物 | Chlordimeform | HCID 22544 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178426111 | HCID 178426111 | — |
反応手順
To a sodium methoxide solution prepared by dissolving 19 grams of sodium metal in 250 milliliters of methanol was added 56 grams of hydroxylamine:hydrochloride in 300 milliliters of methanol. To the resulting mixture was added 98 grams (0.5 mole) of N,N-dimethyl-N'-(4-chloro-2-methylphenyl)methanimidamide. The mixture was stirred at room temperature for 18 hours. The solid reaction product was recovered by filtration and the filtrate concentrated by evaporation under reduced pressure. The residue and the solid reaction product (filter cake) were suspended in water, collected by filtration, water washed and recrystallized from ethanol. The N-(4-chloro-2-methylphenyl)-N'-hydroxymethanimidamide product was recovered in a yield of 81.7 grams (89% of theoretical) and melted at 171°-171.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04237168 |
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| 出典データセット | uspto-grants-1980_12 |
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| ORD ID | ord-dbd04e5c2d42444180cea3c79f92479a |
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| 出典メモ | uspto-grants-1980_12 |
|---|