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o-Anisohydrazide → Methyl 4-{1,1-difluoro-2-[2-(2-methoxybenzoyl)hydrazino]-2-oxoethyl}benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | o-Anisohydrazide | HCID 24051 | — |
| 反応物 | 3-(Ethyliminomethylideneamino)propyl-dimethylazanium chloride | HCID 5351932 | — |
| 反応物 | 2-(4-(Methoxycarbonyl)phenyl)-2,2-difluoroacetic acid | HCID 57541239 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 4-{1,1-difluoro-2-[2-(2-methoxybenzoyl)hydrazino]-2-oxoethyl}benzoate | HCID 57541230 | — |
反応手順
To a solution of difluoro[4-(methoxycarbonyl)phenyl]acetic acid (0.12 g, 0.52 mmol) and 2-methoxybenzohydrazide (0.13 g, 0.78 mmol) in methylene chloride (2 mL) was added 3-{[(ethylimino)methylene]amino}-N,N-dimethylpropan-1-aminium chloride (0.2 g, 1.04 mmol). The resulting solution was stirred at ambient temperature for 16 hours. The reaction was purified by flash chromatography (0-4% methanol/methylene chloride) to give methyl 4-{1,1-difluoro-2-[2-(2-methoxybenzoyl)hydrazino]-2-oxoethyl}benzoate as a white solid. ESIMS calcd 379.1 (M++H), found 379.1 (M++H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08026260B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-bf22575aacab48e994ccef9098e2f592 |
| 出典メモ | uspto-grants-2011_09 |