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Dimethylformamide → Cyano-acetic acid 1-butoxycarbonyl-ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Butyl Lactate | HCID 8738 | — |
| 反応物 | Cyanoacetic acid | HCID 9740 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Cyano-acetic acid 1-butoxycarbonyl-ethyl ester | HCID 23325215 | — |
反応手順
A mixture of 292.32 g of butyllactate, 204.14 g of cyanoacetic acid, and 14.66 g of 4-dimethylaminopyridine (DMAP) in 2000 ml of CH2Cl2 was stirred in a 3 L three-neck round bottom flask equipped with a mechanical stirrer. About 50 ml of N-N′-dimethylformide (DMF) was added to make a clear solution. The above clear solution was chilled in an ice water bath. A separately prepared dicyclohexylcarbodiimide (DCC) solution (495.19 g in 500 ml CH2Cl2) was added to the above chilled solution by using an addition funnel. White precipitate formed within five minutes after the start of the addition. The reaction mixture was left stirred overnight.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07534907B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-67c5ae4431a242f190b4c1a3875e1265 |
| 出典メモ | uspto-grants-2009_05 |