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Potassium Carbonate → (S)-2-[(5-Chloro-pyrimidin-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 | 2,5-Dichloropyrimidine | HCID 590641 | — |
| 反応物 | tert-Butyl (2S)-2-(aminomethyl)pyrrolidine-1-carboxylate | HCID 1512533 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | (S)-2-[(5-Chloro-pyrimidin-2-ylamino)-methyl]-pyrrolidine-1-carboxylic acid tert-butyl ester | HCID 67090501 | 48.6% |
反応手順
(S)-2-Aminomethylpyrrolidine-1-carboxylic acid tert-butyl ester (3.38 g), 2,5-dichloropyrimidine (2.50 g), potassium carbonate (4.67 g) and diisopropylethylamine (8.79 ml) were heated in xylene (60 ml) at 100° C. for 3.75 h. The cooled reaction mixture was filtered and the filtrate evaporated to a gum which was chromatographed on silica gel, eluting with ethyl acetate-pentane fractions, to afford the title compound as a pale yellow solid (2.55 g). Mass Spectrum (API+): Found 213 (MH+-tBoc). C14H2135ClN4O2 requires 312.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741329B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-ef0d216aaeaa4a9c9e8bedfec0dcb933 |
| 出典メモ | uspto-grants-2010_06 |