関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | L-Proline | HCID 145742 | — |
| 反応物 | 2-Morpholinoethylamine | HCID 408285 | — |
| 反応物 | tert-Butyl 3-iodobenzylcarbamate | HCID 11645663 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | [3-(2-Morpholin-4-yl-ethylamino)-benzyl]-carbamic acid isopropyl ester | HCID 67415913 | 76.3% |
反応手順
A mixture of (3-iodo-benzyl)-carbamic acid tert-butyl ester (272 mg, 0.816 mmol), 4-(2-aminoethyl)morpholine (0.16 mL, 1.225 mmol), K2CO3 (232 mg, 1.679 mmol), CuI (19 mg, 0.10 mmol), L-proline (19 mg, 0.163 mmol) and DMSO (5 mL) was heated at 85° C. for 1 h. The reaction was cooled, poured onto water and the aqueous layer extracted with EtOAc (×3). The organic layers were combined and washed with water, brine and dried (Na2SO4). Chromatography (MeOH/EtOAc) afforded [3-(2-morpholin-4-yl-ethylamino)-benzyl]-carbamic acid isopropyl ester (200 mg) as an orange viscous oil. m/z (M+1) 336.16.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08044041B2 |
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| 出典データセット | uspto-grants-2011_10 |
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| ORD ID | ord-b1b0976911de4e949281075102bade76 |
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| 出典メモ | uspto-grants-2011_10 |
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