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Sulfuric Acid → Fmoc-Cys(Trt)-OMe
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | N-((9H-Fluoren-9-ylmethoxy)carbonyl)-S-(triphenylmethyl)-L-cysteine | HCID 128239 | — |
| 反応物 | (R)-methyl 2-amino-3-(tritylthio)propanoate | HCID 10429690 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Fmoc-Cys(Trt)-OMe | HCID 59278482 | — |
反応手順
and H2N-Cys(Trt)-OMe 26. 7.2 g (12.3 mmol) of Fmoc-Cys(Trt)-OH was dissolved in 70 ml of MeOH and added 1.5 ml of conc. sulfuric acid. The reaction mixture was refluxed for 4 hr, the solvent was removed. The mixture was then mixed with ethyl acetate, and washed with water, saturated NaHCO3, and brine. Removing the solvent under vacuum gave 25 as a white foamy solid. The crude product was dissolved in 20 ml of 20% piperidine solution in DMF. After 2 hr, the solvent was removed. Silicagel chromatography (CH2Cl2:MeOH=10:1) gave 4.0 g (86% two step yield) of 26 as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07172905B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-7139a46faeff436eb41454de270b5363 |
| 出典メモ | uspto-grants-2007_02 |