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Tetrahedron Letters
Volumn 55, Issue 3, 2014, Pages 623-628
Heterogeneous reusable catalyst, ultrasound energy, and no solvent: A quick and green recipe for one-pot synthesis of β-phosphonomalononitriles at room temperature
Author keywords

Clays; Crystallization; Heterogeneous catalysis; Phosphonates; Ultrasound irradiation
Indexed keywords

BETA PHOSPHONOMALNITRILE; NITRILE; UNCLASSIFIED DRUG;
EID: 84891830451     PISSN: 00404039     EISSN: 18733581     Source Type: Journal    
DOI: 10.1016/j.tetlet.2013.11.095     Document Type: Article
Times cited : (18)
References (53)
  • 52
    • 84891826953 scopus 로고    scopus 로고
    • 2O product. The freshly prepared HPA was dissolved in 150 mL water and added dropwise to 500 mL aqueous suspension of 10 mg montmorillonite KSF (stirred for 3 h)
    • 2O product. The freshly prepared HPA was dissolved in 150 mL water and added dropwise to 500 mL aqueous suspension of 10 mg montmorillonite KSF (stirred for 3 h). This mixture was stirred for 5 h and the water was evaporated over water bath to get a dry powder, which was kept overnight in air oven at 110 C. A portion of this solid was then calcined at 425 C for 3 h to get a heteropoly acid clay nano-composite and was named HCNC-1. Catalysts named as HCNC-2, HCNC-3, and HCNC-4 were also prepared in the same manner by using only 50% HPA loading of that used in the preparation of HCNC-1 on montmorillonite-KSF, kaolin, and montmorillonite-K10 respectively and HPA-5 contains only 25% loading of the as prepared HPA on montmorillonite-KSF.
  • 53
    • 84891832591 scopus 로고    scopus 로고
    • General procedure for the synthesis of β-phosphonomalononitriles: A mixture of an aldehyde (1 equiv), malononitrile (1 equiv), triethylphosphite (1.5 equiv), and the catalyst (0.1 equiv) was taken in a 5 ml glass test tube with a total reaction volume of 0.4-0.5 ml approximately. The reaction mixture was placed at room temperature for appropriate time period under ultrasonic irradiation, performed in a Bandelin Sonorex Super RK 510 H ultrasonic bath with inner tank dimensions; l × w × d: 300 × 240 × 150 mm, exterior dimensions; l × w × h: 325 × 265 × 305 mm, frequency: 35 kHz and ultrasonic peak output: 640 Wâ̂-. After completion of the reaction (monitored by TLC), the mixture was dissolved in ethyl acetate and filtered to separate the catalyst. The catalyst was subsequently washed with ethyl acetate, dried, and reused several times under same reaction conditions. Filtrate was worked up in ethyl acetate: water (1:1) system
    • 4 and concentrated under reduced pressure. The crude products were purified by the crystallization technique and no column purification was followed. IR spectra were recorded on Perkin-Elmer IR spectrophotometer. ESI-MS and HRMS spectra were recorded on Agilent 1100 LC and HRMS-6540-UHD machines. NMR spectra were recorded on Brucker-Advance DPX FT-NMR 400 MHz instrument.

* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.