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Chloroacetyl chloride → 2-Chloromethyl-3-(2-chlorophenyl)-5-methyl-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-methylbenzamide | HCID 16785685 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Chloromethyl-3-(2-chlorophenyl)-5-methyl-3H-quinazolin-4-one | HCID 22316547 | 24% |
反応手順
Prepared according to Procedure B with 1g (2.18 g, 8.36 mmol) and chloroacetyl chloride (2.0 mL, 25.1 mmol) in acetic acid (40 mL). Purified by two chromatographies in CH2Cl2 and EtOAc/hexanes, followed by recrystallization from isopropanol to afford 638 mg of an off-white crystalline solid (24%). 1H NMR (DMSO-d6) δ: 7.73-7.80 (m, 3H); 7.58-7.64 (m, 3H); 7.41 (d, J=7.4 Hz, 1H); 4.40 (d, J=12 Hz, 1H), 4.26 (d, J=12 Hz, 1H); 2.74 (s, 3H). MS (ES): m/z 319.0 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06667300B2 |
| 出典データセット | uspto-grants-2003_12 |
| ORD ID | ord-f24e4bfdc626405bb11daae8cb29a575 |
| 出典メモ | uspto-grants-2003_12 |