関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methylhydrazine | HCID 6061 | — |
| 反応物 | Dimethyl acetylenedicarboxylate | HCID 12980 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 178498595 | HCID 178498595 | — |
反応手順
102.3 g (0.72 mol) Dimethyl acetylenedicarboxylate was added to 1000 ml ether and the mixture cooled to -5° C. in an ice-methanol bath. 33 g (0.72 mol) methylhydrazine in 100 ml ether was added dropwise at a rate that the inner temperature did not rise above 0° C. The mixture was stirred for one hour at 0° C., the precipitate suction filtered off, washed with ether and dried at 40° C. in vacuo. The intermediate was immersed in an oil-bath heated to 120° C. The reaction product was recrystallised from methanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05869686 |
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| 出典データセット | uspto-grants-1999_02 |
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| ORD ID | ord-c57b0a82a8434593bae231040cfa0921 |
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| 出典メモ | uspto-grants-1999_02 |
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