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HRID 641728作成日:2026年10月26日

Triphenylphosphine → 4-(2-Chloro-5-methoxyanilino)-5,7-di-(3-morpholinopropoxy)quinazoline

https://huagongshe.com/reaction/641728

反応式

関与物質

役割名称HCID仕込み量
反応物TriphenylphosphineHCID 11776—
反応物Di-tert-butyl azodicarboxylateHCID 97268—
反応物3-Morpholino-1-propanolHCID 199576—
反応物4-(2-Chloro-5-methoxyanilino)-7-hydroxy-5-(3-morpholinopropoxy)quinazolineHCID 135830916—
溶媒DichloromethaneHCID 6344—
生成物4-(2-Chloro-5-methoxyanilino)-5,7-di-(3-morpholinopropoxy)quinazolineHCID 987287231.1%

反応手順

Di-tert-butyl azodicarboxylate (0.035 g) was added dropwise to a stirred mixture of 4-(2-chloro-5-methoxyanilino)-7-hydroxy-5-(3-morpholinopropoxy)quinazoline (0.045 g), 4-(3-hydroxypropyl)morpholine (0.016 g), triphenylphosphine (0.04 g) and methylene chloride (1 ml). The reaction mixture was stirred at ambient temperature for 10 minutes. The mixture was evaporated and the residue was purified by column chromatography on silica using a 9:10:1 mixture of methylene chloride, ethyl acetate and a saturated methanolic ammonia solution as eluent. The material so obtained was triturated under diethyl ether. The resultant solid was isolated, washed with diethyl ether and dried under vacuum to give the title compound (0.018 g); NMR Spectrum: (DMSOd6 and CF3COOD) 2.2-2.4 (m, 4H), 3.15 (m, 4H), 3.35 (m, 4H), 3.5 (m, 4H), 3.7 (m, 4H), 3.8 (s, 3H), 4.02 (t, 4H), 4.35 (t, 2H), 4.6 (t, 2H), 6.95 (s, 1H), 7.03 (s, 1H), 7.05 (m, 1H), 7.5 (s, 1H), 7.6 (d, 1H), 8.88 (s, 1H); Mass Spectrum: M+H+ 572 and 574.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07696214B2
出典データセットuspto-grants-2010_04
ORD IDord-7bc1fc9474d94880a94c1a237b3ee5e0
出典メモuspto-grants-2010_04