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Dicyclohexylcarbodiimide → (R)-quinuclidin-3-yl 2-(4-chlorophenylamino)-2-phenylacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 3-Quinuclidinol, (-)- | HCID 91404 | — |
| 反応物 | (4-Chloro-phenylamino)-phenyl-acetic acid | HCID 305145 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (R)-quinuclidin-3-yl 2-(4-chlorophenylamino)-2-phenylacetate | HCID 46840420 | 37.5% |
反応手順
To a solution of (4-chloro-phenylamino)-phenyl-acetic acid (I28) (574 mg, 2.20 mmol) in dry THF (20 mL), are added DCC (543 mg, 2.64 mmol), HOBt (359 mg, 2.64 mmol) and 3(R)-quinuclidinol (558 mg, 4.40 mmol). The resulting mixture is stirred at RT overnight (UPLC-MS monitoring: complete conversion). The solvent is evaporated and the residue is portitioned between EtOAc and 2M K2CO3. The organic phase is dried over Na2SO4, filtered and evaporated to dryness. The resulting crude is purified by flash chromatography (DCM/MeOH=99/1 to 85/15) to obtain the title compound as a white solid (306 mg, 37% yield, mixture of diastereoisomers).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835682B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-ec2ac91b91924a1c803577c4259fa398 |
| 出典メモ | uspto-grants-2014_09 |