pentylhydrazine

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

实验步骤: A warm solution of 6.02 g (49.3 mM) ethoxymethylenemalononitrile in 20 ml of ethanol was added via a cannula to a stirred solution of 6.04 g (59.1 mM)n- pentylhydrazine in 20 ml of ethanol at 50° C. The reaction mixture was then heated to reflux for 30 minutes, then cooled in a refrigerator for 18 hours. The off-white crystalline precipitate was filtered to yield 7.73 g (88%) of the title compound, mp=143°-144° C.; tlc, Rf =0.5, silica gel, methanol:chloroform (1:19). The reaction mixture was then heated to reflux for 30 minutes cooled in a refrigerator for 18 hours The off-white crystalline precipitate was filtered

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

实验步骤: A warm solution of 6.02 g (49.3 mM) ethoxymethylenemalononitrile in 20 ml of ethanol was added via a cannula with stirring to a solution of 6.04 g (59.1 mM) of pentylhydrazine in 20 ml ethanol maintained at 50°. The mixture was then heated to reflux for 30 minutes, then cooled in a refrigerator (ca 3°) for 18 hours. The white crystalline precipitate was filtered to afford 7.73 g (88%) of the title compound; mp, 143°-144°; tlc, Rf =0.50, silica gel, methanol:chloroform (1:19). maintained at 50° The mixture was then heated to reflux for 30 minutes cooled in a refrigerator (ca 3°) for 18 hours The white crystalline precipitate was filtered

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

实验步骤: A warm solution of 6.02 g (49.3 mM) ethoxymethylenemalononitrile in 20 ml of ethanol was added via a cannula with stirring to a solution of 6.04 g (59.1 mM) of pentylhydrazine in 20 ml ethanol maintained at 50°. The mixture was then heated to reflux for 30 minutes, then cooled in a refrigerator (ca 3°) for 18 hours. The white crystalline precipitate was filtered to afford 7.73 g (88%) of the title compound; mp, 143°-144°; tlc, Rf =0.50, silica gel, methanol:chloroform (1:19). maintained at 50° The mixture was then heated to reflux for 30 minutes cooled in a refrigerator (ca 3°) for 18 hours The white crystalline precipitate was filtered

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

实验步骤: A warm solution of 6.02 g (49.3 mM) ethoxymethylenemalononitrile in 20 ml of ethanol was added via a cannula to a stirred solution of 6.04 g (59.1 mM)n- pentylhydrazine in 20 ml of ethanol at 50° C. The reaction mixture was then heated to reflux for 30 minutes, then cooled in a refrigerator for 18 hours. The off-white crystalline precipitate was filtered to yield 7.73 g (88%) of the title compound, mp=143°-144° C.; tlc, Rf =0.5, silica gel, methanol:chloroform (1:19). The reaction mixture was then heated to reflux for 30 minutes cooled in a refrigerator for 18 hours The off-white crystalline precipitate was filtered

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a magnetically stirred solution of oxo-acetic acid ethyl ester (35.08 ml, 177 mmol; 50% solution in toluene) in ethanol (450 ml) was added n-pentylhydrazine (21.7 g, 212 mmol) and the resulting solution was heated at 80° C. for 16 hours. The obtained mixture was allowed to attain room temperature and concentrated. The resulting residue was taken up in ethylacetate and water. The organic layer was separated and subsequently dried over MgSO4, filtered and concentrated to give (pentylhydrazono)acetic acid ethyl ester (Intermediate II-1) (32.2 gram, 93% yield) as a purple colored oil. 1H-NMR (400 MHz, CDCl3) δ 0.87-0.94 (m, 3H), 1.25-1.42 (m, 7H), 1.55-1.68 (m, 2H), 3.17-3.23 (m, 1H), 3.35-3.45 (m, 1H), 4.28 (q, J=7, 2H), 6.51 (br s, 1H), 6.72 (s, 1H). to attain room temperature concentrated The organic layer was separated subsequently dried over MgSO4 filtered concentrated

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

实验步骤: A warm solution of 6.02 g (49.3 mM) ethoxymethylenemalononitrile in 20 ml of ethanol was added via a cannula to a stirred solution of 6.04 g (59.1 mM)n-pentylhydrazine in 20 ml of ethanol at 50° C. The reaction mixture was then heated to reflux for 30 minutes, then cooled in a refrigerator for 18 hours. The off-white crystalline precipitate was filtered to yield 7.73 g (88%) of the title compound, mp=143°-144° C.; tlc, Rf =0.5, silica gel, methanol: chloroform (1:19). The reaction mixture was then heated to reflux for 30 minutes cooled in a refrigerator for 18 hours The off-white crystalline precipitate was filtered

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

实验步骤: A warm solution of 6.02 g (49.3 mM) ethoxymethylenemalononitrile in 20 ml of ethanol was added via a cannula with stirring to a solution of 6.04 g (59.1 mM) of pentylhydrazine in 20 ml ethanol maintained at 50°. The mixture was then heated to reflux for 30 minutes, then cooled in a refrigerator (ca 3°) for 18 hours. The white crystalline precipitate was filtered to afford 7.73 g (88%) of the title compound; mp, 143°-144°; tlc, Rf =0.50, silica gel, methanol:chloroform (1:19). maintained at 50° The mixture was then heated to reflux for 30 minutes cooled in a refrigerator (ca 3°) for 18 hours The white crystalline precipitate was filtered

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

实验步骤: A warm solution of 6.02 g (49.3 mM) ethoxymethylenemalononitrile in 20 ml of ethanol was added via a cannula to a stirred solution of 6.04 g (59.1 mM)n- pentylhydrazine in 20 ml of ethanol at 50° C. The reaction mixture was then heated to reflux for 30 minutes, then cooled in a refrigerator for 18 hours. The off-white crystalline precipitate was filtered to yield 7.73 g (88%) of the title compound, mp=143°-144° C.; tlc, Rf =0.5, silica gel, methanol:chloroform (1:19). The reaction mixture was then heated to reflux for 30 minutes cooled in a refrigerator for 18 hours The off-white crystalline precipitate was filtered