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Chloroacetyl chloride → 2-Chloromethyl-3-(2-chlorophenyl)-5-fluoro-3H-quinazolin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | 2-amino-N-(2-chlorophenyl)-6-fluorobenzamide | HCID 22316568 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Chloromethyl-3-(2-chlorophenyl)-5-fluoro-3H-quinazolin-4-one | HCID 22316567 | 70.4% |
反応手順
Prepared according to Procedure B with 1e (500 mg, 1.89 mmol) and chloroacetyl chloride (0.45 mL, 5.67 mmol) in acetic acid (10 mL). Purified by extraction from aq. K2CO3 and recrystallization from isopropanol to afford 430 mg of an off-white crystalline solid (70%). 1H NMR (CDCl3) δ: 7.76 (dt, J=5.3, 8.2 Hz, 1H); 7.56-7.65 (m, 2H); 7.47-7.56 (m, 3H); 7.16-7.25 (m, 1H); 4.35 (d, J=12 Hz, 1H), 4.07 (d, J=12 Hz, 1H). MS (ES): m/z 323.0 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653077B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-4926188f0c694731908c918c24a1219d |
| 出典メモ | uspto-grants-2014_02 |