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Methyl 3-amino-2-chloro-5-fluoro-4-methylbenzoate → 2,3-Dichloro-5-fluoro-4-methylbenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 3-amino-2-chloro-5-fluoro-4-methylbenzoate | HCID 13657452 | — |
| 反応物 | Hydrochloride sodium nitrite | HCID 86602196 | — |
| 触媒 | Cuprous chloride | HCID 62652 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 2,3-Dichloro-5-fluoro-4-methylbenzoic acid | HCID 13657441 | — |
反応手順
8 g of methyl 3-amino-2-chloro-5-fluoro-4-methylbenzoate are diazotized with NaNO2 /HCl in aqueous solution. This diazonium salt solution is added dropwise to a solution of 4.1 g of CuCl in 16 ml of concentrated HCl. The mixture is then warmed until no further gas is formed. After cooling, the solid which has precipitated is separated off and taken up in 30 ml of 50% strength EtOH. After addition of 2.3 g of NaOH, the mixture is boiled for 1 hour. After cooling to room temperature, the mixture is acidified with HCl and the solid which has precipitated is isolated. Melting point: 179°-80°. Yield: 5.2 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04762844 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-b8e48d4c300a4eb88eedc02c00b64818 |
| 出典メモ | uspto-grants-1988_08 |