関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl 2-[(2,6-dichlorobenzyl)amino]-3-(4-nitrophenyl)propanoate | HCID 11269078 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 11302630 | HCID 11302630 | — |
反応手順
To methyl 2-[(2,6-dichlorobenzyl)amino]-3-(4-nitrophenyl)propanoate 7a (8.2 g) solubilized in CH3COOH in an ultrasonic bath is added PtO2 hydrate (typical Pt content 79-84%) (0.02 g). A H2 pressure of 15 psi is then applied at RT and consumed after 5 min. An other H2 pressure of 10 psis is then applied at RT and consumed after 5-10 min. A H2 pressure of 10 psis is again applied at RT and a stabilization is observed after 5 min. The catalyst is filtered over celite under nitrogen and washed with CH3COOH. The solvent is evaporated. AcOEt (200 ml) is added to the residue and this organic phase is washed three times with saturated NaHCO3 (200 ml), dried over MgSO4 and evaporated. The residue is purified by silica gel chromatography using CH2Cl2/CH3OH/NH4OH cc (99.75/0.25/0.025) as eluent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07638630B2 |
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| 出典データセット | uspto-grants-2009_12 |
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| ORD ID | ord-66d3d69161b541ca8addcd5fcf33d69f |
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| 出典メモ | uspto-grants-2009_12 |
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