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Chlorosuccinimide → (4R,9aR)-7-Chloro-4,6-dimethyl-3,4,9,9a-tetrahydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | (R)-4,6-Dimethyl-3,4-dihydro-1H-2,4a,5-triaza-fluorene-2-carboxylic Acid Tert-butyl Ester | HCID 69357516 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (4R,9aR)-7-Chloro-4,6-dimethyl-3,4,9,9a-tetrahydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester | HCID 69357620 | — |
反応手順
To a solution of 0.20 g (0.66 mmol) (R)-4,6-dimethyl-3,4-dihydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester in 2 mL tetrahydrofuran was added 92.1 μg (0.69 mmol) N-chlorosuccinimide. The reaction was stirred at 50 deg C. for 18 h, then the solvent was evaporated and the residue was purified by column chromatography on silica gel (0.032–0.063 mm) with ethyl acetate:dichloromethane (1:19) as eluant.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07208494B2 |
| 出典データセット | uspto-grants-2007_04 |
| ORD ID | ord-3aa9b957890b4570a1b952d8a8cb99f4 |
| 出典メモ | uspto-grants-2007_04 |