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Chloroacetyl chloride → 5-Chloro-2-chloromethyl-3-o-tolyl-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-6-chloro-N-o-tolylbenzamide | HCID 12487367 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-Chloro-2-chloromethyl-3-o-tolyl-3H-quinazolin-4-one | HCID 12487373 | 37% |
反応手順
Prepared according to Procedure B with 1j (750 mg, 2.88 mmol) and chloroacetyl chloride (0.69 mL, 8.63 mmol) in acetic acid (15 mL). Purified by chromatography in CH2Cl2, followed by recrystallization from isopropanol to afford 340 mg of a white solid (37%). 1H NMR (CDCl3) δ: 7.69 (d, J=2.1 Hz, 1H); 7.68 (q, J=7.4 Hz, 1H); 7.54 (dd, J=2.2, 7.0 Hz, 1H); 7.35-7.47 (m, 3H); 7.21-7.25 (m, 1H); 4.27 (d, J=12 Hz, 1H); 4.11 (d, J=12 Hz, 1H); 2.18 (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 | US08653077B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-bd13829226874b17ab82e0b7b324b7f7 |
| 出典メモ | uspto-grants-2014_02 |