関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-2-(phenylmethylidene)hydrazine | HCID 66691978 | — |
| 触媒 | 1,1-Dimethylhydrazine | HCID 5976 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-1-methyl-2-(phenylmethylidene)hydrazine | HCID 66691562 | 99.4% |
反応手順
To a 50 mL volume three-necked flask, 1.0 g of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-2-(phenylmethylidene)hydrazine ((40-a)-(14)-6), 3.5 ml of toluene and 629 mg of potassium carbonate were added and then, 9.1 mg of N,N-dimethylhydrazine solved in 2.3 ml of toluene and 577 mg of dimethyl sulfate were added thereto at 5° C. The mixture was stirred at 5° C. for 24 hours, 3 g of water was added thereto and the organic layer was removed. The aqueous layer was extracted with 3.5 ml of toluene two times. The organic layers were combined and concentrated under reduced pressure to give 1.037 g of a mixture (19:1 (GC area %)) of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-1-methyl-2-(phenylmethylidene)hydrazine ((40-b)-(15)-5) and methyl 2-(2,6-diethyl-4-methylphenyl)-2-oxo-N-(phenylmethylidene)ethanehydrazonate (x-1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08884010B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-2132c99abdb14d6b9427369704835bb5 |
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| 出典メモ | uspto-grants-2014_11 |
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