関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Isocyanate | HCID 12228 | — |
| 反応物 | Gyki-53405 | HCID 126756 | — |
| 反応物 | Calcium hydride | HCID 3033859 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | HCID 23190221 | HCID 23190221 | 82.4% |
反応手順
0.70 g (2 mmol) of the product of Example 15 was dissolved in benzene dehydrated over calcium hydride, 0.3 ml (5 mmol) of methyl isocyanate was added and the reaction mixture was stirred at 50° C. for 4 hours. The crystals formed after coling were filtered, washed with 3×3 ml of benzene, then triturated with 20 ml of hot benzene. The hot mixture was filtered, the precipitate was washed with 3×3 ml of benzene and dried to give 0.65 g (79.6%) of the aimed product, m.p.: 168°-170° C. (decomp.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05519019 |
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| 出典データセット | uspto-grants-1996_05 |
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| ORD ID | ord-b328d1cb071b4b6d8536b28243674b35 |
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| 出典メモ | uspto-grants-1996_05 |
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