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Chloroacetyl chloride → 2-chloro-N-(2,4-dihydroxyphenyl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | 4-Aminobenzene-1,3-diol hydrochloride | HCID 13408822 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-chloro-N-(2,4-dihydroxyphenyl)acetamide | HCID 52904873 | — |
反応手順
To a solution of 4-aminoresorcinol hydrochloride (30 g, 0.1857 mol) in CH2Cl2, (460 mL) TEA (77.6 mL, 0.557 mol) was added at 0° C. To the resulting mixture, chloroacetyl chloride (14.78 mL, 0.1857 mol) was added drop wise and the solution was stirred for 60 h at RT. The crude product was washed through a plug of silica gel with CH2Cl2 and purified through column chromatography using 100% CH2Cl2→25%→50%→75% 90:10:1 CH2Cl2:MeOH:NH4OH. The solution was concentrated in vacuo to give the title compound. MS (ESI, pos. ion) m/z: 202 (M+1). Mass calc'd for C8H8ClNO3: 201.02.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07435823B2 |
| 出典データセット | uspto-grants-2008_10 |
| ORD ID | ord-2c7662f64c0949ce9647e4d5e59ff243 |
| 出典メモ | uspto-grants-2008_10 |