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Potassium Carbonate → (S)-2-[(5-Cyano-pyridin-2-ylamino)-methyl]-pyrrolidine-1-carboxylic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | tert-Butyl (2S)-2-(aminomethyl)pyrrolidine-1-carboxylate | HCID 1512533 | — |
| 反応物 | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | (S)-2-[(5-Cyano-pyridin-2-ylamino)-methyl]-pyrrolidine-1-carboxylic acid tert-butyl ester | HCID 67090650 | 44.2% |
反応手順
(S)-2-Aminomethyl pyrrolidine-1-carboxylic acid tert-butyl ester (0.3 g), 6-chloronicotinonitrile (0.21 g), potassium carbonate (0.41 g) and diisopropylethylamine (0.78 ml) were heated in xylene at 130° C. for 26 h, cooled and the mixture filtered through kieselguhr. The filtrate was evaporated and the residue chromatographed on silica gel, eluting with ethyl acetate-hexane mixtures to afford the title compound (0.2 g). Mass Spectrum (API+): Found 303 (MH+). C16H22N4O2 requires 302.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07919507B2 |
| 出典データセット | uspto-grants-2011_04 |
| ORD ID | ord-061c4cdc5dc1458cb796d5a8c1b40da4 |
| 出典メモ | uspto-grants-2011_04 |