The Studies of Microwave Effects on the Chemical Reactions

Journal of the Chinese Chemical Society

Volumn 44, Issue 3, 1997, Pages 169-182

  Chen, Shui Tein ^a   Tseng, Ping Hui ^b   Yu, Hui Ming ^a   Wu, Chi Yue ^a   Hsiao, Kwo Feng ^a   Wu, Shih Hsiung ^a   Wang, Kung Tsung ^a,b  

^a INSTITUTE OF BIOLOGICAL CHEMISTRY   (Taiwan)

^b NATIONAL TAIWAN UNIVERSITY   (Taiwan)

Author keywords

Enzymatic catalysis; Hydrolysis; Microwave irradiation; Molecular agitation; Peptide bond; Rate enhancement; Saponification; Specific cleavage

Indexed keywords

EID: 0001079022     PISSN: 00094536     EISSN: None     Source Type: Journal    
DOI: 10.1002/jccs.199700028     Document Type: Article

References (55)

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29. In a typical reaction, to amino acid on HMP-resin (0.5 gr, ca. 0.25 meq. of amino acid) suspended in dimethylformamide (10 mL) was added 3.0 equ. (0.75 mmol) of symmetric anhydride or of the preformed N-protected amino acid active ester. Nitrogen gas was bubbled through the side-arm into the reaction vessel and served as a stirrer. The reaction was conducted via microwave irradiation for 2-6 minutes and stopped by filtering off the reaction solution via the side-arm. Small amounts of the sample with resin were taken for ninhydrine test. Then, Fmoc-Ala (3 equ.), DCC (3 equ) was added and reacted at room temperature for 6 hours. The product was cleaved from the resin using trifluoroacetic acid (Cleavage conditions followed the procedure of the Howard Florey Fmoc Workshop Manual (1985) by J. Wade & G. Tregear or see Applied Biosystem User's Manual, p. 2-21.). The purity of product was measured by HPLC analysis, and the peak identification was compared with the authentic sample.
30. In a typical reaction, to amino acid on HMP-resin (0.5 gr, ca. 0.25 meq. of amino acid) suspended in dimethylformamide (10 mL) was added 3.0 equ. (0.75 mmol) of symmetric anhydride or of the preformed N-protected amino acid active ester. Nitrogen gas was bubbled through the side-arm into the reaction vessel and served as a stirrer. The reaction was conducted via microwave irradiation for 2-6 minutes and stopped by filtering off the reaction solution via the side-arm. Small amounts of the sample with resin were taken for ninhydrine test. Then, Fmoc-Ala (3 equ.), DCC (3 equ) was added and reacted at room temperature for 6 hours. The product was cleaved from the resin using trifluoroacetic acid (Cleavage conditions followed the procedure of the Howard Florey Fmoc Workshop Manual (1985) by J. Wade & G. Tregear or see Applied Biosystem User's Manual, p. 2-21.). The purity of product was measured by HPLC analysis, and the peak identification was compared with the authentic sample.
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44. In this study, approximately 10% of full power (i.e., 72 W) was used. For the preparative scale reaction, a Synthewave 402 microwave oven (Prolabo, France) was used, and the temperature of the reaction solution was maintained at 45°C.
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