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Potassium Carbonate → 4-[(2-tert-Butoxycarbonylamino-ethyl)-(4-fluoro-benzyl)-amino]-but-2-enoic Acid Methyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Butenoic acid, 4-bromo-, methyl ester | HCID 5369175 | — |
| 反応物 | tert-Butyl (2-((4-fluorobenzyl)amino)ethyl)carbamate | HCID 69655592 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 4-[(2-tert-Butoxycarbonylamino-ethyl)-(4-fluoro-benzyl)-amino]-but-2-enoic Acid Methyl Ester | HCID 69655603 | 89.2% |
反応手順
[2-(4-Fluoro-benzylamino)-ethyl]-carbamic acid tert-butyl ester (7.0 g, 26.1 mmol) and potassium carbonate (7.2 g, 52.2 mmol) were stirred in acetone (150 mL). A mixture of methyl 4-bromocrotonate (4.7 g, 26.1 mmol, 3.1 mL) in acetone (50 mL) was added to this solution dropwise using an addition funnel. After 18 h the solution was filtered, concentrated and chromatographed on silica gel to yield the title compound as a yellow oil (8.53 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07098212B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-e4d1881149c74c9fa1f7a0ec43dc4d6d |
| 出典メモ | uspto-grants-2006_08 |