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4-Methylmorpholine → 4-(Methyloxycarbonyl)benzoyl-2(S)-phenylsulfonylamino-beta-alanine t-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 反応物 | 2-Methylterephthalic acid | HCID 228086 | — |
| 反応物 | (S)-3-amino-2-benzenesulfonylamino-propionic acid tert-butyl ester hydrochloride | HCID 22853534 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(Methyloxycarbonyl)benzoyl-2(S)-phenylsulfonylamino-beta-alanine t-butyl ester | HCID 86751098 | — |
反応手順
A slurry of mono-methyl terephthalic acid (32-1, Aldrich) (0.25 g, 1.4 mmol) and 19-2a (0.5 g, 1.4 mmol) in acetonitrile (7 mL) was treated with N-methyl morpholine (0.31 mL, 2.8 mmol) and BOP reagent (0.62 g, 1.4 mmol) for 24 h. The solution was diluted with EtOAc, washed with H2O, 10% KHSO4, saturated NaHCO3 and brine. The organic layer was dried over MgSO4, filtered and evaporated to give a tan solid. Column chromatography (40% EtOAc/Hexanes) gave 32-2 as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05648368 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-112c5f47032b47e4a4a80acb7046b6b1 |
| 出典メモ | uspto-grants-1997_07 |