Chloroacetyl chloride → 5-Chloro-2-chloromethyl-3-(2-methoxyphenyl)-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-(2-methoxyphenyl)benzamide	HCID 22316549	—
溶媒	Acetic Acid	HCID 176	—
生成物	5-Chloro-2-chloromethyl-3-(2-methoxyphenyl)-3H-quinazolin-4-one	HCID 22316590	28%

反応手順

Prepared according to Procedure B with 1l (2.6 g, 9.41 mmol) and chloroacetyl chloride (2.2 mL, 28.2 mmol) in acetic acid (40 mL). Purified by chromatography in CH2Cl2, followed by recrystallization from isopropanol to afford 874 mg of a pale yellow solid (28%). 1H NMR (CDCl3) δ: 7.55-7.74 (m, 2H); 7.47-7.54 (m, 2H); 7.34 (dd, J=1.7, 7.8 Hz, 1H); 7.13 (dt, J=1.2, 7.7 Hz, 1H); 7.08 (dd, J=1.0, 8.4 Hz, 1H); 4.29 (d, J=12 Hz, 1H); 4.11 (d, J=12 Hz, 1H); 3.80 (s, 3H). MS (ES): m/z 335.0 (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-c4b552d6bd4447b6a2a1207c3ac4b14b
出典メモ	uspto-grants-2013_07