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Acetone → Phthalidyl 2-chloro-3-pyridinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Chloronicotinic acid | HCID 76258 | — |
| 反応物 | 1(3H)-Isobenzofuranone, 3-bromo- | HCID 96218 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Phthalidyl 2-chloro-3-pyridinecarboxylate | HCID 12673421 | 67% |
反応手順
To 600 ml of acetone, 31.5 g of 2-chloro-3-pyridinecarboxylic acid is added and suspended by stirring. Triethylamine (40 ml) is added and after 30 minutes 42.6 g of 3-bromophthalide is poured with stirring into the resulting reaction mixture. The mixture is refluxed for 4 hours and then poured into 2000 ml of water at 50° C. To obtain a precipitated compound, the reaction mixture is cooled with continuous stirring. The solid precipitate is collected by filtration, washed with cooled water and then dried under vacuum at a temperature of 40° C. A yield of 38.7 g (67% of theory) of phthalidyl 2-chloro-3-pyridinecarboxylate is obtained (m.p. 137°-8° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04255581 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-9a92ca4fd2b946499350958549e3da98 |
| 出典メモ | uspto-grants-1981_03 |