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Chloroform → 2-amino-N-(2-chlorophenyl)-5-hydroxybenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | 2-Chloroaniline | HCID 7240 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 5-Hydroxyanthranilic acid | HCID 164592 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-amino-N-(2-chlorophenyl)-5-hydroxybenzamide | HCID 22316564 | 12% |
反応手順
Prepared according to Procedure A using 2-amino-5-hydroxybenzoic acid (5.0 g, 32.7 mmol) and SOCl2 (6.0 mL, 81.6 mmol) in benzene (150 mL), followed by 2-chloroaniline (6.9 mL, 65.4 mmol) and CHCl3 (150 mL). The product was purified by two chromatographies in MeOH/CH2Cl2 to provide 990 mg of a brown solid (12%). 1H NMR (MeOH-d4) δ: 7.92 (dd, J=1.6, 8.1 Hz, 1H); 7.48 (dd, J=1.5, 7.7 Hz, 1H); 7.34 (dt, J=1.5, 7.7 Hz, 1H); 7.20 (dt, J=1.7, 7.7 Hz, 1H); 7.16 (d, J=2.7 Hz, 1H); 6.83 (dd, J=2.7, 8.7 Hz, 1H); 6.76 (d, J=8.7 Hz, 1H); [6.24 (br s, 2H)). MS (ES): m/z 263.0 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08623881B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-9dddfc8a55334d2d85257dc006101e77 |
| 出典メモ | uspto-grants-2014_01 |