2-ethylbenzohydrazide

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of immino ether (85 mg, 0.474 mmoles) and 2-ethyl benzo-hydrazide (164 mg, 1 mmole) in acetonitrile (0.5 mL), was warmed under reflux. After 1 hour stirring, solvent was distilled and substituted by 2-ethoxyethanol (0.6 mL). The reaction mixture was refluxed for 3 hours, the solvent evaporated under vacuum and the residue, re-dissolved in CH2Cl2 (2 mL), was chromatographed on a silica gel column (10 g). As elution solvents, mixtures of CH2Cl2 and CH3COOC2H5 in varying proportion (99:1 to 95:5) were used. Fractions containing the desired product were collected, solvent evaporated to give 96,27 mg (72.6%) of compound (XIII). Of particular interest, was compound (XIV), which, can be synthesised according to the procedure hereafter reported in example 2. was warmed under reflux solvent was distilled The reaction mixture was refluxed for 3 hours the solvent evaporated under vacuum the residue, re-dissolved in CH2Cl2 (2 mL) was chromatographed on a silica gel column (10 g) As elution solvents, mixtures of CH2Cl2 and CH3COOC2H5 Fractions containing the desired product were collected solvent evaporated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of immino ether (85 mg, 0.474 mmoles) and 2-ethyl benzo-hydrazide (164 mg, 1 mmole) in acetonitrile (0.5 mL), was warmed under reflux. After 1 hour stirring, solvent was distilled and substituted by 2-ethoxyethanol (0.6 mL). The reaction mixture was refluxed for 3 hours, the solvent evaporated under vacuum and the residue, re-dissolved in CH2Cl2 (2 mL), was chromatographed on a silica gel column (10 g). As elution solvents, mixtures of CH2Cl2 and CH3COOC2H5 in varying proportion (99:1 to 95:5) were used. Fractions containing the desired product were collected, solvent evaporated to give 96,27 mg (72.6%) of compound (XIII). Of particular interest, was compound (XIV), which, can be synthesised according to the procedure hereafter reported in example 2. was warmed under reflux solvent was distilled The reaction mixture was refluxed for 3 hours the solvent evaporated under vacuum the residue, re-dissolved in CH2Cl2 (2 mL) was chromatographed on a silica gel column (10 g) As elution solvents, mixtures of CH2Cl2 and CH3COOC2H5 Fractions containing the desired product were collected solvent evaporated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of immino ether (85 mg, 0.474 mmoles) and 2-ethyl benzo-hydrazide (164 mg, 1 mmole) in acetonitrile (0.5 mL), was warmed under reflux. After 1 hour stirring, solvent was distilled and substituted by 2-ethoxyethanol (0.6 mL). The reaction mixture was refluxed for 3 hours, the solvent evaporated under vacuum and the residue, re-dissolved in CH2Cl2 (2 mL), was chromatographed on a silica gel column (10 g). As elution solvents, mixtures of CH2Cl2 and CH3COOC2H5 in varying proportion (99:1 to 95:5) were used. Fractions containing the desired product were collected, solvent evaporated to give 96,27 mg (72.6%) of compound (XIII). Of particular interest, was compound (XIV), which, can be synthesised according to the procedure hereafter reported in example 2. was warmed under reflux solvent was distilled The reaction mixture was refluxed for 3 hours the solvent evaporated under vacuum the residue, re-dissolved in CH2Cl2 (2 mL) was chromatographed on a silica gel column (10 g) As elution solvents, mixtures of CH2Cl2 and CH3COOC2H5 Fractions containing the desired product were collected solvent evaporated