3-octyloxolane-2,5-dione

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 3-(3,5-di-t-butyl-4-hydroxyphenyl)propanoic acid hydrazide (12.1 g, 41.1 mmol), 2-octylsuccinic anhydride (9.0 g, 41.1 mmol) and 20 ml of toluene was refluxed for one hour under a nitrogen atmosphere with the azeotropic removal of water (Dean-Stark assembly). The solvent was removed under vacuum while heating the reaction mass. 18.7 g of a very viscous, clear yellow liquid was obtained. The solvent was removed under vacuum while heating the reaction mass 18.7 g of a very viscous, clear yellow liquid was obtained

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 3-(3,5-di-t-butyl-4-hydroxyphenyl)propanoic acid hydrazide (12.1 g, 41.1 mmol), 2-octylsuccinic anhydride (9.0 g, 41.1 mmol) and 20 ml of toluene was refluxed for one hour under a nitrogen atmosphere with the azeotropic removal of water (Dean-Stark assembly). The solvent was removed under vacuum while heating the reaction mass. 18.7 g of a very viscous, clear yellow liquid was obtained. The solvent was removed under vacuum while heating the reaction mass 18.7 g of a very viscous, clear yellow liquid was obtained

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 10 parts n-octylsuccinic anhydride and 12 parts tris(hydroxymethyl)aminomethane were heated neat 3 hrs. at 180° C. under a rapid flow of N2. The product was obtained as a colorless glass in 100% yield. The following spectral properties confirm the structure shown below: ir (neat) 3300 (OH), 1600 (C=N); nmr (CDCl3) δ 4.40 (broad s, 4.0 H, 2 CH2 's in rings), δ 4.25 (broad s, 3.7 H, 4 OH, addition of D2O eliminates peak), δ 3.55 (broadened 10 Hz AB, 7.2 H, 4 CH2O), δ 2.5 (broad s, 3.0 H, CH--CH), δ 1.4 (broad s with t shoulder at 0.9, 17 H, n-C8H17). at 180° C. The product was obtained as a colorless glass in 100% yield

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 10 parts n-octylsuccinic anhydride and 12 parts tris(hydroxymethyl)aminomethane were heated neat 3 hrs. at 180° C. under a rapid flow of N2. The product was obtained as a colorless glass in 100% yield. The following spectral properties confirm the structure shown below: ir (neat) 3300 (OH), 1600 (C=N); nmr (CDCl3) δ 4.40 (broad s, 4.0 H, 2 CH2 's in rings), δ 4.25 (broad s, 3.7 H, 4 OH, addition of D2O eliminates peak), δ 3.55 (broadened 10 Hz AB, 7.2 H, 4 CH2O), δ 2.5 (broad s, 3.0 H, CH--CH), δ 1.4 (broad s with t shoulder at 0.9, 17 H, n-C8H17). at 180° C. The product was obtained as a colorless glass in 100% yield

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 3-(3,5-di-t-butyl-4hydroxyphenyl)propanoic acid hydrazide (I2.1 g, 41.1 mmol), 2-octylsuccinic anhydride (9.0 g, 41.1 mmol) and 20 ml of toluene was refluxed for one hour under a nitrogen atmosphere with the azeotropic removal of water (Dean-Stark assembly). The solvent was removed under vacuum while heating the reaction mass. 18.7 g of a very viscous, clear yellow liquid was obtained. The solvent was removed under vacuum while heating the reaction mass 18.7 g of a very viscous, clear yellow liquid was obtained

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: n-Octylsuccinyl dichloride was prepared by reacting n-octylsuccinic anhydride with PCl5 at 105°-110° C. for about four hours. After working the product up 101.3 g of liquid was obtained which had a purity of 84.3% according to chloride content. The corrected yield was 79.2%. at 105°-110° C. for about four hours was obtained which

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: n-Octylsuccinyl dichloride was prepared by reacting n-octylsuccinic anhydride with PCl5 at 105°-110° C for about four hours. After working the product up 101.3 g of liquid was obtained which had a purity of 84.3% according to chloride content. The corrected yield was 79.2%. at 105°-110° C for about four hours was obtained which

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 3-(3,5-di-t-butyl-4-hydroxyphenyl)propanoic acid hydrazide (12.1 g, 41.1 mmol), 2-octylsuccinic anhydride (9.0 g, 41.1 mmol) and 20 ml of toluene was refluxed for one hour under a nitrogen atmosphere with the azeotropic removal of water (Dean-Stark assembly). The solvent was removed under vacuum while heating the reaction mass. 18.7 g of a very viscous, clear yellow liquid was obtained. The solvent was removed under vacuum while heating the reaction mass 18.7 g of a very viscous, clear yellow liquid was obtained

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 10 parts n-octylsuccinic anhydride and 12 parts tris(hydroxymethyl)aminomethane were heated neat 3 hrs. at 180° C. under a rapid flow of N2. The product was obtained as a colorless glass in 100% yield. The following spectral properties confirm the structure shown below: ir (neat) 3300 (OH), 1600 (C=N); nmr (CDCl3) δ 4.40 (broad s, 4.0 H, 2 CH2 's in rings), δ 4.25 (broad s, 3.7 H, 4 OH, addition of D2O eliminates peak), δ 3.55 (broadened 10 Hz AB, 7.2 H, 4 CH2O), δ 2.5 (broad s, 3.0 H, CH--CH), δ 1.4 (broad s with t shoulder at 0.9, 17 H, n-C8H17). at 180° C. The product was obtained as a colorless glass in 100% yield