(2.0 mL). The reaction mixture was stirred atroom temperaturefor one hour and monitored by TLC. Then the solvent was evaporated in vacuo to give the crude material, which was purified viasilica gelcolumn chromatography using PE/EtOAc (2:1) to obtain3a(64.4 mg, 90% yield) as a light ...
Demixing effects in thin-layer chromatography have been investigated with NH 2 -modified silica gel precoated plates and for frequently used hydroorganic binary solvents of various compositions with salt addition.The position of the solvent demixing front depends on: (1) solvent composition, (2) ...
The solution was impregnated on silica gel, evaporated to dryness and the residue was chromatographed on a silica gel column. Elution with a mixture of hexane (75%) and toluene (25%) gave first a pale yellow solution of unreacted compounds. Elution with a mixture of hexane (25%) and ...
COLUMN LIQUID CHROMATOGRAPHYCOLUMN PACKINGSSILICA GELPOROUS CARBONLow-temperature T 1 relaxation measurements of a proton pseudo-spin glass system in mixed rubidium-ammonium dihydrogen arsenate crystals are presented. The experimentally observed features of the magnetization decay in the rotating frame are ...
(Beijing, China), was used to purify compounds isolated from atmospheric silica gel column chromatography. A Pursuit XRs 10 C18 column (250 × 21.2 mm) was used for preparative HPLC. Preparative medium performance liquid chromatography (MPLC) was carried out on an octadecylsilyl C18 column (25 ...
Reactions of 1 with methylamine and ethylamine give the corresponding amidines 10-RNHC(Me)=NH-7,8-C2B9H11 (R = Me (6) and Et (7)) as mixtures of E- and Z-isomers, which cannot be separated by column chromatography on silica (Scheme 3). Scheme 3. Synthesis of amidines 10-MeNHC(...
Reactions of 1 with methylamine and ethylamine give the corresponding amidines 10-RNHC(Me)=NH-7,8-C2B9H11 (R = Me (6) and Et (7)) as mixtures of E- and Z-isomers, which cannot be separated by column chromatography on silica (Scheme 3). Scheme 3. Synthesis of amidines 10-MeNHC(...
Flash column chromatography was performed on Silica Gel 60 Å (Merck KGaA, Darmstadt, Germany). Vacuum distillation was performed in a Büchi Model B580 GKR oven (Büchi Labortechnik AG, Flawil, Switzerland). Thin-layer chromatography was carried out on Silica Gel plates (Merck Kieselgel 60 F...
Flash column chromatography was performed on Silica Gel 60 Å (Merck KGaA, Darmstadt, Germany). Vacuum distillation was performed in a Büchi Model B580 GKR oven (Büchi Labortechnik AG, Flawil, Switzerland). Thin-layer chromatography was car- ried out on Silica Gel plates (Merck Kieselgel 60...