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Hydrochloric Acid → Diisopropyl Ether
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 2-Chloroethyl chloroformate | HCID 12305 | — |
| 反応物 | 4-Aminohydratropic acid | HCID 43026 | — |
| 反応物 | Trisodium phosphate dodecahydrate | HCID 61473 | — |
| 生成物 | Diisopropyl Ether | HCID 7914 | — |
| 生成物 | 2-(4-{[(2-Chloroethoxy)carbonyl]amino}phenyl)propanoic Acid | HCID 18423575 | — |
反応手順
1 g (6 mmol) of 2-(4-aminophenyl)propanoic acid was suspended in 30 ml of dichloromethane and 1.24 ml (12 mmol) of 2-chloroethylchloroformate were added at 0° C. under stirring. After 30 minutes at the same temperature 2.27 g (6 mmol) of sodium phosphate dodecahydrate were added portionwise. After 4 hours the reaction was complete (HPLC-MS). The mixture was made acidic by using hydrochloric acid 0.5N and the product extracted with dichloromethane. The organic layer was dried over sodium sulphate and evaporated under vacuum. 1.4 g (100%yield) of the title compound were obtained by crystallization from diisopropylether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06455559B1 |
| 出典データセット | uspto-grants-2002_09 |
| ORD ID | ord-b8fe52451ece4672826b8d63fb756574 |
| 出典メモ | uspto-grants-2002_09 |