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Toluene → 3-Anilino-4-isopropoxycarbonyl-5-methylpyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Isopropyl chloroacetate | HCID 7759 | — |
| 反応物 | Hydrazinecarbothioamide, N-phenyl- | HCID 730679 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Anilino-4-isopropoxycarbonyl-5-methylpyrazole | HCID 20475386 | — |
反応手順
35.7 g of isopropyl 2-chloroacetate is added to a suspension of 33.5 g of 4-phenylthiosemicarbazide in 150 ml of tetrahydrofuran. After the mixture has been stirred for 30 minutes it is boiled for a further 30 minutes and then allowed to cool. The precipitated solid is isolated by suction filtering, washed with acetone and the residue is heated in a water/acetone mixture (1:1). After the separated sulfur has been poured off, the whole is allowed to cool and is neutralized with aqueous NaHCO3, solution and the precipitated solid is isolated; m.p. 138°-139° C. (from toluene).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04260775 |
| 出典データセット | uspto-grants-1981_04 |
| ORD ID | ord-d16790c1377a4c428b0eea47a823bc70 |
| 出典メモ | uspto-grants-1981_04 |