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Triethylamine → Coumate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Chlorosulfamic acid | HCID 24499 | — |
| 反応物 | 4-Methylumbelliferone | HCID 5280567 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Coumate | HCID 9859866 | 41.1% |
反応手順
A slurry of 7-hydroxy-4-methylcoumarin (17.6 g, 0.10 mole) in acetonitrile (100 ml) was treated with a total of 84 ml of 3M sulfamoyl chloride (0.255 mole) in acetonitrile. The mixture was then treated dropwise with triethylamine (25.8 g, 0.255 mole). The reaction temperature was allowed to rise to 45° without any cooling. The mixture was stirred overnight at ambient temperature. The precipitate was collected, triturated with water, and dried in a vacuum oven at 70° C. for 15 hr to give 10.5 g (41%) of white powder, mp 161°-164° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05194446 |
| 出典データセット | uspto-grants-1993_03 |
| ORD ID | ord-626cd38e37d4499f901cda7c0758e833 |
| 出典メモ | uspto-grants-1993_03 |