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Water → Phenyl (4-chloro-2-cyanophenyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 反応物 | 2-Amino-5-chlorobenzonitrile | HCID 80019 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | Phenyl (4-chloro-2-cyanophenyl)carbamate | HCID 66877344 | — |
反応手順
(Step 1) To a solution of 2-amino-5-chlorobenzonitrile (5.0 g) and dimethylaminopyridine (0.12 g) in dimethylacetamide (25 ml) was added dropwise phenyl chlorocarbonate (6.2 ml) at room temperature, and the mixture was stirred overnight. The reaction mixture was poured into water, and extracted twice with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and filtered. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5-*3:7) to give phenyl (4-chloro-2-cyanophenyl)carbamate (7.04 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08481569B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-12c4fe8d2eb34c0e938d9981a8796f9c |
| 出典メモ | uspto-grants-2013_07 |