関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | L-Tyrosine, N-(1,1-dimethylethoxy)carbonyl- | HCID 117439 | — |
| 生成物 | N-Boc-N-methyl-4-methoxy-L-phenylalanine | HCID 7016369 | 95% |
反応手順
6.0 g of NaH suspension were washed by decantation 3 times with PE, 50 ml of THF were poured on, and the mixture was cooled to 0° C. Then 32 mmol of BOC-L-tyrosine dissolved in 110 ml of THF were slowly added dropwise, and subsequently 16 ml of methyl iodide were added. The suspension was stirred at RT with exclusion of light for 25 h, 50 ml of EA were added, and the mixture was cautiously hydrolyzed with water. It was concentrated under reduced pressure to a small volume, EA was added, and the mixture was acidified with 2N KHSO4. After extraction with EA, the organic phases were washed with 10% strength sodium thiosulfate solution, dried (MgSO4) and evaporated under reduced pressure. Yield: 95%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05504189 |
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| 出典データセット | uspto-grants-1996_04 |
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| ORD ID | ord-c86972516fab465e8b0ba5ccbb34a320 |
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| 出典メモ | uspto-grants-1996_04 |
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