関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Malonamide | HCID 7911 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | 2-(3,4-Dichlorophenoxy)-3-(dimethylamino)prop-2-enal | HCID 54555818 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 5-(3,4-Dichlorophenoxy)-2-hydroxy-3-pyridinecarboxamide | HCID 178513692 | 43.5% |
反応手順
2-(3,4-Dichlorophenoxy)-3-dimethylaminopropenal (13 g), malonamide (5.6 g), and t-BuOK (6.2 g) were mixed in 50 ml of DMSO and heated at 45° C. for 30 minutes. This mixture was then stirred at room temperature for an additional 24 hours after which it was poured into 200 g of an ice-water mixture and acidified with concentrated HCl. A solid formed which was collected by centrifugation, vacuum dried, and recrystallized from 2-propanol to give 6.5 g of the desired 5-(3,4-dichlorophenoxy)-2-hydroxy-3-pyridinecarboxamide, m.p. 246°-249° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04558134 |
|---|
| 出典データセット | uspto-grants-1985_12 |
|---|
| ORD ID | ord-46b63bdf1795404aa60e604ba73f7f82 |
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| 出典メモ | uspto-grants-1985_12 |
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