関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Benzyl bromoacetate | HCID 62576 | — |
| 反応物 | N-[(Phenylmethoxy)carbonyl]-L-tyrosine methyl ester | HCID 7010613 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 15003986 | HCID 15003986 | 72.7% |
反応手順
Under ice-cooling condition, to 25 ml of DMF solution containing 5.70 g of Z-Tyr-OCH3 was added 692 mg of sodium hydride (containing 60%) and the mixture was stirred for 30 minutes, then 3.96 g of benzyl bromoacetate was added thereto and the whole mixture was stirred at 50° C. for 1 hour. The reaction mixture was concentrated under reduced pressure and the residue thus obtained was extracted with 100 ml of ethyl acetate. The ethyl acetate layer was washed with water and a saturated sodium chloride aqueous solution twice, respectively, then dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue thus obtained was added to a silica gel column and eluted with petroleum ether-chloroform (1:4) to obtain 6.00 g (yield: 72.6%) of the above-mentioned objective product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05204326 |
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| 出典データセット | uspto-grants-1993_04 |
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| ORD ID | ord-83a3949ee7314cb38bfe64930f149b01 |
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| 出典メモ | uspto-grants-1993_04 |
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