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Methyl propiolate → HCID 178498875、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl propiolate | HCID 13536 | — |
| 反応物 | p-Methoxybenzamidoxime | HCID 21471 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178498875 | HCID 178498875 | 30.1% |
反応手順
A solution of methyl propiolate (25.4 g, 0.3 mol), p-methoxybenzamidoxime (50 g, 0.3 mol) and CH3OH (700 ml) was heated at reflux with stirring. After 8 hours, the reaction mixture was concentrated to dryness, and the residue treated with diphenyl ether (300 ml) and heated at reflux. After 2.5 hours, the reaction mixture was poured in C6H14 (2 L) and allowed to stand. The C6H14 was decanted off and the residue chromatographed on silica gel. The product was eluted with 2% CH3OH--CHCl3 to yield 21 g (30%) of 63; m.p. 188°-90° C. (trituration with Et2O). Analysis calculated for C12H12N2O3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04853383 |
| 出典データセット | uspto-grants-1989_08 |
| ORD ID | ord-8bd343e28517496b939e0886d5fa72f4 |
| 出典メモ | uspto-grants-1989_08 |