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Water → methyl N-{2-[4-(1-methylpropoxy)phenoxy]ethyl}carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl (2-chloroethyl)carbamate | HCID 251614 | — |
| 反応物 | 4-(1-Methyl-1-propyloxy)-phenol | HCID 13882004 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | methyl N-{2-[4-(1-methylpropoxy)phenoxy]ethyl}carbamate | HCID 15662569 | — |
反応手順
A mixture of 4-(1-methylpropoxy)phenol (9.2 mmol), methyl 2-chloroethylcarbamate (11.9 mmol), and potassium carbonate (18.4 mmol) in 20 ml of dimethylformamide (DMF) is heated at 85° for 18 hours. The reaction mixture is cooled to room temperature (RT), poured into water and extracted with ether. The combined ether extracts are washed with water until neutral, followed with brine and dried over calcium sulfate. The solvent is removed in vacuo and the residue is placed under high vacuum at 80° for ca. 2 hours to remove the excess methyl 2-chloroethylcarbamate. Purification by preparative thin layer chromatography (prep. TLC) gives methyl N-{2-[4-(1-methylpropoxy)phenoxy]ethyl}carbamate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04697033 |
| 出典データセット | uspto-grants-1987_09 |
| ORD ID | ord-add4aaf646714895ab7b855a5ef88067 |
| 出典メモ | uspto-grants-1987_09 |