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Pyridine → Carbamic acid, (2-fluoro-2-oxoethyl)-, 9H-fluoren-9-ylmethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Cyanuric fluoride | HCID 12664 | — |
| 反応物 | Fmoc-Gly-OH | HCID 93124 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Carbamic acid, (2-fluoro-2-oxoethyl)-, 9H-fluoren-9-ylmethyl ester | HCID 11011991 | — |
反応手順
FMOC-Glycine (5.02 g, 16.82 mmol) (Bachem) was dissolved in dichloromethane (85 mL). Pyridine (1.36 mL, 16.82 mmol) (Aldrich) and cyanuric fluoride (2.27 g, 16.82 mmol) (Aldrich) were successively added at room temperature and the mixture was stirred overnight. Ice cold water (100 mL) was added and the resulting slurry was filtered. The filtrate was poured into a separatory funnel and the layers were separated. The organic layer was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to afford FMOC-glycyl fluoride as a white powder. (Yield 3.67 g, 73%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084270B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-8e925202aa5c48a68b53aa693faeea25 |
| 出典メモ | uspto-grants-2006_08 |