化工社化工社 化学情報印刷レポート · 研究参考用
Ethyl chloroformate → Ethyl trans-2-phenylcyclopropanecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | trans-2-Phenylcyclopropanecarboxylic acid | HCID 237413 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Ethyl trans-2-phenylcyclopropanecarboxylate | HCID 252496 | — |
反応手順
To an ice cold solution of 1.62 g of (1R, 2R)-2-phenyl-cyclopropane carboxylic acid (from racemic trans-2-phenyl-cyclopropane carboxylic acid by resolution on a chiral HPLC column) and 2.0 mL of triethylamine and 0.12 g of 4-dimethylaminopyridine was added 1.2 mL of ethyl chloroformate The mixture was allowed to warm and stir for 1 h, then washed with 25 mL of 3N HCl, 25 mL of water, 25 mL of saturated sodium carbonate and dried over magnesium sulfate. Removal of solvents under reduced pressure gave 1.9 g of product as an oil: MS (m+1)=191.1; 1H NMR (400 MHz, CDCl3) 7.3 (dd, 2H), 7.2 (t, 1H), 7.1 (d, 2H), 4.18 (q, 2H), 2.5 (m, 1H), 1.9 (m, 1H), 1.6 (m, 1H), 1.3 (overlapping m and t, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07452893B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-0463f58e7f0f455a947cb6e71379836b |
| 出典メモ | uspto-grants-2008_11 |