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3-Nitrobenzaldehyde → [Hydroxy-(3-nitro-phenyl)methyl]-phosphonic acid dimethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Nitrobenzaldehyde | HCID 7449 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Dimethylphosphite | HCID 21884954 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | [Hydroxy-(3-nitro-phenyl)methyl]-phosphonic acid dimethyl ester | HCID 11299958 | 77% |
反応手順
3-Nitrobenzaldehyde (20 g, 0.132 mol) was dissolved in 100 mL of ethyl acetate. Triethylamine (22 mL, 0.158 mol, 1.2 eq) was added, followed by dimethylphosphite (15.7 mL, 0.171 mmol, 1.3 eq) and the mixture was stirred at room temperature. After 2 hours the mixture was diluted with 150 mL of ethyl acetate and washed with saturated aqueous ammonium chloride (2×50 mL) and water (50 mL). The organic layer was dried over Na2SO4 and concentrated under reduced pressure. The residue was treated with ethyl ether to obtain a beige solid, which was filtered and dried under vacuum at 40° C. for 1 h (26.7 g, 77% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541575B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-6b6d0775abb64f6ba1883c5aa00c22cb |
| 出典メモ | uspto-grants-2013_09 |