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Volumn , Issue 1, 2008, Pages 0105-0107

Applications of lanthanide trichloride hydrates, prepared from mischmetall, in the Biginelli reaction

a CNRS (France)

Author keywords

Biginelli type reaction; Lanthanide trichlorides; Mischmetall

Indexed keywords

ALLOY; LANTHANIDE; LANTHANIDE TRICHLORIDE; MISCHMETALL; UNCLASSIFIED DRUG;

ARTICLE; BIGINELLI REACTION; CATALYST; CHEMICAL REACTION; SYNTHESIS;

EID: 38549112888 PISSN: 09365214 EISSN: None Source Type: Journal
DOI: 10.1055/s-2007-992387 Document Type: Article

Times cited : (25)

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- Typical Experimental Procedure for Biginelli Reaction: A mixture of ethyl acetoacetate (638 μL, 5 mmol, urea (451 mg, 7.5 mmol) or thiourea (571 mg, 7.5 mmol, aldehyde (5 mmol, LnCl3·7H2O (Ln, mischmetall, 373 mg, 1 mmol, 0.2 equiv) and 12 M HCl acid (1 drop) in absolute EtOH (10 mL) was placed under magnetic stirring and refluxed in EtOH for 5 h. The reaction mixture was then cooled to r.t. and poured onto an ice-water mixture (25 g, The solution was stirred for 5 min until a solid appeared. The precipitate was then filtered and the solid was washed with cold H2O (2 x, then with an EtOH-H2O mixture (1:1, 2 x) and finally dried under vacuum. The crude product was then purified by recrystallization in absolute EtOH. Selected Spectral Data for 6-Methyl-2-oxo-4-phenyl-1,2,3,4-tetrahydropyrimidine-5-carboxylic Acid Ethyl Ester (1, colorless crystals; mp 207-209°C lit.8 mp 206-209°C, yield: 1.954
- +, 307.1 (35).

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