化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → n-Formyl-l-leucine tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (Formyloxy)acetonitrile | HCID 4205685 | — |
| 反応物 | tert-butyl (2S)-2-amino-4-methylpentanoate hydrochloride | HCID 12451443 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | n-Formyl-l-leucine tert-butyl ester | HCID 11160222 | — |
反応手順
The preparation was performed in analogy to W. Duczek et al., Synthesis, 37-38 (1996). A solution of 4.04 g (40 mmol) of triethylamine in 10 mL of dichloromethane was added to a solution of 8.94 g (40 mmol) of L-leucine tert-butyl ester hydrochloride and 3.4 g (40 mmol) of cyanomethyl formate in 60 mL of dichloromethane at 0° C. The reaction solution was allowed to warm to room temperature, stirred at room temperature overnight, and then washed twice with saturated NaCl solution. The phases were separated and the organic phase was dried over magnesium sulfate. The residue obtained after filtration and removal of the solvent in vacuo was distilled in vacuo. Yield: 7.5 g (87%). Boiling point: 118° C./2.7 Pa (0.02 torr).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06794517B2 |
| 出典データセット | uspto-grants-2004_09 |
| ORD ID | ord-9e9028be0e544e89848222ce1c80d7fa |
| 出典メモ | uspto-grants-2004_09 |