関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl cyclopropane-1,1-dicarboxylate | HCID 73790 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 1-(hydroxymethyl)cyclopropane-1-carboxylate | HCID 12450336 | — |
反応手順
In accordance with the method described in the document (Tetrahedron Letters, 40, 5467 (1988)), a solution of 720 mg of 1-hydroxymethyl-cyclopropane carboxylic acid ethyl ester obtained from 1,1-cyclopropane dicarboxylic acid diethyl ester in 10 mL of dichloromethane was added with 1.05 mL of triethylamine and 0.5 mL of methanesulfonyl chloride under ice cooling, and stirred at this temperature for 2 hours. After adding water, the reaction solution was extracted with ethyl acetate. The organic layer was washed successively with 1N hydrochloric acid, saturated brine, saturated aqueous sodium hydrogen carbonate and saturated brine. The organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated, to afford 1.04 g of the title compound as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07429609B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-920abec18a3340b0b66b7d0f175cbe10 |
|---|
| 出典メモ | uspto-grants-2008_09 |
|---|