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	US06800620B2
出典データセット	uspto-grants-2004_10
ORD ID	ord-ca44cf57b37144028377924f175c5245
出典メモ	uspto-grants-2004_10