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	US08492389B2
出典データセット	uspto-grants-2013_07
ORD ID	ord-ef8cdc8aa52741e7a7b3ea5820a2dd1d
出典メモ	uspto-grants-2013_07