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Ethanol → HCID 178481914、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | O-(6-Chlorobenzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate | HCID 42624899 | — |
| 反応物 | (2R,4R)-4-amino-5-(3'-chlorobiphenyl-4-yl)-2-hydroxypentanoic acid ethyl ester | HCID 86682253 | — |
| 反応物 | HCID 178481916 | HCID 178481916 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178481914 | HCID 178481914 | 14.4% |
反応手順
5-Hydroxy-1-methyl-1H-pyrazole-3-carboxylic acid (19.6 mg, 138 μmol) was combined with HCTU (56.9 mg, 138 μmol) in DMF. The mixture was stirred for 10 minutes at room temperature before adding DIPEA (72 μL, 413 μmol) and (2R,4R)-4-amino-5-(3′-chlorobiphenyl-4-yl)-2-hydroxypentanoic acid ethyl ester (50 mg, 0.1 mmol). The resulting mixture was stirred overnight at room temperature. EtOH (402 μL, 6.9 mmol) and 1 M LiOH in water (1.1 mL, 1.1 mmol) was added and the mixture was stirred at room temperature for 1 hour. The mixture was evaporated under reduced pressure and purified by preparative HPLC to yield the title compound (6.4 mg). MS m/z [M+H]+ calc'd for C22H22ClN3O5, 444.12. found 444.4.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09108934B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-98d8baac5d6e4b2896a34a4c3ad1f125 |
| 出典メモ | uspto-grants-2015_08 |