関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | N-[(1S)-1-(4-bromophenyl)ethyl]cyclopropanecarboxamide | HCID 800360 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | Ferrocene-1,1'-bis-(diphenylphosphine) | HCID 635956 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (S)-Cyclopropanecarboxylic acid [1-(4-formyl-phenyl)-ethyl]-amide | HCID 118940157 | — |
反応手順
To 5.0 g (19 mmol) (S)-cyclopropanecarboxylic acid [1-(4-bromo-phenyl)-ethyl]-amide (WO 2012/01107) in 40 mL MeOH are added 125 mg (0.600 mmol) palladium-(II)-acetate, 620 mg (1.10 mmol) 1,1′-bis(diphenylphosphino)-ferrocene and 4.6 g (56 mmol) sodium acetate. The mixture is stirred at 100° C. and 5 bar CO atmosphere over night. After that time, the mixture is filtered over celite and the filtrate is concentrated by evaporation. The residue is purified by column chromatography (silica gel; gradient hexane/EtOAc 1:0→1:4) to yield the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09340510B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-1979cb4f0c68403c9e15e365b6562dbe |
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| 出典メモ | uspto-grants-2016_05 |
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