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Triethylamine → Tert-butyl 3-(6-chloro-4-iodopyridin-2-ylamino)cyclohexylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Di-tert-butyl dicarbonate | HCID 90495 | — |
| 反応物 | N1-(6-chloro-4-iodopyridin-2-yl)cyclohexane-1,3-diamine | HCID 86649873 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Tert-butyl 3-(6-chloro-4-iodopyridin-2-ylamino)cyclohexylcarbamate | HCID 87185034 | 53.3% |
反応手順
To a mixture of Example 260a (2.60 g, 7.39 mmol) and triethylamine (1.340 mL, 9.61 mmol) in tetrahydrofuran (50 mL) was added BOC2O (1.78 g, 8.13 mmol) at 0° C. The ice bath was removed and the reaction was stirred at room temperature for 90 minutes. The reaction was diluted with EtOAc and washed with brine and sat. NaHCO3. The organic layer was dried over MgSO4, filtered, concentrated, and purified on an 80 g column using the ISCO Companion flash system eluting with hexane/EtOAc (8:2 to 6:4) to give 1.78 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08435980B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-42e50410994c467c8e7938d88b5ad25f |
| 出典メモ | uspto-grants-2013_05 |