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DL-alanine → 2-(Cyclopentylformamido)propanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | DL-alanine | HCID 602 | — |
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Cyclopentanecarbonyl chloride | HCID 78284 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(Cyclopentylformamido)propanoic acid | HCID 12621980 | — |
反応手順
16.8 g (0.189 mol) of D,L-alanine and 41.98 g (0.415 mol) of triethylamine are initially charged in 200 ml of dichloromethane. At 0° C. 45.07 g (0.415 mol) of trimethylsilyl chloride are added dropwise, and the mixture is stirred at room temperature for 1 h and then at 40° C. for 1 h. The solution is cooled to −10° C., and 25 g (0.189 mol) of cyclopentanecarbonyl chloride are added dropwise. The mixture is stirred at −10° C. for 2 h and at room temperature for 1 h. With ice-cooling, 100 ml of water are added dropwise, the mixture is stirred for 10 min. and the resulting precipitate is filtered off with suction. The precipitate is washed with 300 ml of water and then with 300 ml of diethyl ether and subsequently dried at 60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07098207B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-d94f79942acd4abda53fdab727364607 |
| 出典メモ | uspto-grants-2006_08 |