関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Amino-3-cyclopropyl-2-methyl-propionitrile | HCID 84716049 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (1-Cyano-2-cyclopropyl-1-methyl-ethyl)-carbamic acid benzyl ester | HCID 90204034 | 60% |
反応手順
To a solution of 2-Amino-3-cyclopropyl-2-methyl-propionitrile (Example 66a, 5.01 g, 30.9 mmol) in dry THF (119 mL) was added DIEA (12.1 mL, 67.9 mmol) and benzyl carbonochloridate (CAN 501-53-1, 5.57 mL, 37.1 mmol). The reaction was stirred at 45° C. for 18 hours. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in ethylacetate and extracted with an 1.0M aqueous solution of sodium bicarbonate. The organic layer was dried over sodium sulfate and evaporated down to dryness. The crude material was purified by flash chromatography eluting with a gradient of heptane/ethylacetate to yield the title compound (6.2, 60%) as a colorless oil. MS (ESI, m/z): 259.5 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09409866B2 |
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| 出典データセット | uspto-grants-2016_08 |
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| ORD ID | ord-05123ffb9a4543f9a9175e88a87b33c5 |
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| 出典メモ | uspto-grants-2016_08 |
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