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Methyl chloroformate → HCID 86740383、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl chloroformate | HCID 6586 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Ethyl beta-amino-beta-ethoxyacrylate hydrochloride | HCID 53395434 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 86740383 | HCID 86740383 | — |
反応手順
A solution consisting of 96 g of ethyl β-amino-β-ethoxyacrylate hydrochloride, 800 ml of methylene chloride and 120 ml of N-methylmorpholine is warmed to 40°. While stirring there is added dropwise within 2 hours a solution of 65 ml of methyl chloroformate in 350 ml of methylene chloride. After completion of the addition, the mixture is stirred at 40° for a further 2 hours. Thereupon, the resulting salt is filtered off under suction and washed with about 50 ml of methylene chloride. The filtrate is evaporated at 40° in a water-jet vacuum. There is obtained crude methyl[(1-ethoxy-2-ethoxycarbonyl)-ethylidene]carbamate in the form of a pale yellow oil which is used immediately in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04549019 |
| 出典データセット | uspto-grants-1985_10 |
| ORD ID | ord-9784dfae229a4f8299c9b1e165277e01 |
| 出典メモ | uspto-grants-1985_10 |