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3
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0030952762
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Flynn, D. L.; Crich, J. Z.; Devraj, R. V.; Hockerman, S. L.; Parlow, J. J.; South, M. S.; Woodard, S. J. Am. Chem. Soc. 1997, 119, 4874.
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(1997)
J. Am. Chem. Soc.
, vol.119
, pp. 4874
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Flynn, D.L.1
Crich, J.Z.2
Devraj, R.V.3
Hockerman, S.L.4
Parlow, J.J.5
South, M.S.6
Woodard, S.7
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4
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0030607141
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Kaldor, S.W.; Siegel, M. G.; Fritz, J. E.; Dressman, B. A.; Hahn, P. J. Tetrahedron Lett. 1996, 37, 7193.
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(1996)
Tetrahedron Lett.
, vol.37
, pp. 7193
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Kaldor, S.W.1
Siegel, M.G.2
Fritz, J.E.3
Dressman, B.A.4
Hahn, P.J.5
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5
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0033223375
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and references cited therein
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Hudson, D. J. Comb. Chem. 1999, 1, 403 and references cited therein.
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(1999)
J. Comb. Chem.
, vol.1
, pp. 403
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Hudson, D.1
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6
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0004091952
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Katz, E.; Eksteen, R.; Schoenmakers, P.; Miller, N., Eds.; Marcel Dekker: New York and references cited therein.
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Doyle, C. A.; Dorsey, J. G. In Handbook of HPLC; Katz, E.; Eksteen, R.; Schoenmakers, P.; Miller, N., Eds.; Marcel Dekker: New York, 1999; pp. 293-324 and references cited therein.
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(1999)
In Handbook of HPLC
, pp. 293-324
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Doyle, C.A.1
Dorsey, J.G.2
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7
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0343665816
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To a mixture of macroporous highly cross-linked polystyrene beads (1.75 g) in N-methyl pyrrolidine (20 mL) was added tris(2-aminoethyl)amine (3 mL). The mixture was agitated overnight in a heater/shaker at 60°C. The beads were washed three times each with DMF, methanol, methylene chloride, ether and then dried in vacuo.
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To a mixture of macroporous highly cross-linked polystyrene beads (1.75 g) in N-methyl pyrrolidine (20 mL) was added tris(2-aminoethyl)amine (3 mL). The mixture was agitated overnight in a heater/shaker at 60°C. The beads were washed three times each with DMF, methanol, methylene chloride, ether and then dried in vacuo.
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8
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0342795570
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To a sample of Tris resin (approximately 20 mg) was added a 0.025 M solution of trans-β-styrene sulfonyl chloride in acetonitrile. The mixture was shaken overnight at ambient temperature, then spun down in a centrifuge. An aliquot (100 μL) was removed and added to acetonitrile (900 μL). Reverse-phase HPLC was performed and the amount of quenched sulfonyl chloride was calculated from a standard curve.
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To a sample of Tris resin (approximately 20 mg) was added a 0.025 M solution of trans-β-styrene sulfonyl chloride in acetonitrile. The mixture was shaken overnight at ambient temperature, then spun down in a centrifuge. An aliquot (100 μL) was removed and added to acetonitrile (900 μL). Reverse-phase HPLC was performed and the amount of quenched sulfonyl chloride was calculated from a standard curve.
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9
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0343230165
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To a 0.025 M solution of amine (1 mL) was added a 0.050 M solution of sulfonyl chloride (1 mL) and triethyl amine (60 μL). The solution was shaken for two hours before the addition of the Tris resin derived from Argopore-Cl (1.2 equiv. based on the 'rapid quenching' activity). The mixture was shaken for an additional 15 minutes and then spun down in a centrifuge. An aliquot was removed and subjected to reverse-phase HPLC/ELSD to obtain the purity.
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To a 0.025 M solution of amine (1 mL) was added a 0.050 M solution of sulfonyl chloride (1 mL) and triethyl amine (60 μL). The solution was shaken for two hours before the addition of the Tris resin derived from Argopore-Cl (1.2 equiv. based on the 'rapid quenching' activity). The mixture was shaken for an additional 15 minutes and then spun down in a centrifuge. An aliquot was removed and subjected to reverse-phase HPLC/ELSD to obtain the purity.
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10
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0343665815
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The purity of the reaction is in reference to only the amine and sulfonyl chloride. No attempt was made in these experiments to remove the triethylamine and triethylammonium chloride.
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The purity of the reaction is in reference to only the amine and sulfonyl chloride. No attempt was made in these experiments to remove the triethylamine and triethylammonium chloride.
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