関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | N-Hydroxysuccinimide | HCID 80170 | — |
| 反応物 | N-(Triphenylmethyl)glycylglycine | HCID 14217166 | — |
| 反応物 | Phe-Gly-OBzl | HCID 91977316 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Trt-Gly-Gly-Phe-Gly-OBz | HCID 131723527 | — |
反応手順
To 10 ml of dry DMF were added 1.54 g of Trt-Gly-Gly, 0.52 g of N-hydroxysuccinimide and 0.93 g of DCC, followed by effecting a reaction at 4° C. for 3 hours, to thereby obtain a reaction mixture. To the obtained reaction mixture was added a DMF solution containing 2.0 g of Phe-Gly-OBn para-toluenesulfonate synthesized in item (1) and 0.41 g of N-methylmorpholine, which are dissolved in 10 ml of DMF, followed by effecting a reaction at 4° C. for 15 hours, to thereby obtain a reaction mixture. A precipitate contained in the obtained reaction mixture was removed and the resultant solution was evaporated to dryness, to thereby obtain a residue. The obtained residue was purified by silica gel column chromatography (silica gel: Art No. 9365, Silica gel 60, 200-400 mesh, manufactured and sold by E. Merck, Darmstadt, Germany, eluent: chloroform/methanol=20/1), to thereby obtain 1.5 g of Trt-Gly-Gly-Phe-Gly-OBz.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06458347B1 |
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| 出典データセット | uspto-grants-2002_10 |
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| ORD ID | ord-ad867d2c90d8478fa63c44df7dbe56a8 |
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| 出典メモ | uspto-grants-2002_10 |
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