2,6-dimethylheptan-4-ol

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a one liter three-neck flask was mixed 100 g (0.69 moles) of 2,6-dimethyl-4-heptanol and 580 g chloroform. Triethylamine (77.1 g; 6 moles) was added and the reaction mixture cooled to 0° C. Methanesulfonyl chloride (83.4 g; 0.73 moles) was added dropwise, keeping the reaction temperature about 0° C. After holding at about 0° C. for one hour, gas chromatograph (GC) showed less than 5% residual alcohol. the reaction temperature about 0° C

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of CIH-HEAP-OH (5 g, 9.9 mmol), 1,1'-carbonyl diimidazole (2.42 g, 15 mmol) and potassium hydroxide (0.40 g, 7.14 mmol) in toluene (40 ml) was heated at 60° C. for 6 hours and cooled. The reaction mixture was filtered. Diethylene triamine (0.51 g, 4.95 mmol) was added to the filtrate and the reaction mixture heated at 60° C. for 6 hours and cooled. The reaction mixture was filtered, the filtrate was washed with water, dried (MgSO4), filtered and concentrated in vacuo to give CIH-HEAP-DTA-NH as a colorless gum (5.63 g, 98i). A solution of CIH-HEAP-DTA-NH (5.50 g, 4.7 mmol) and succinic anhydride (0.47 g, 4.7 mmol) in toluene (40 ml) was stirred at room temperature or 6 hours. 1,1'-Carbonyl diimidazole (0.77 g, 4.75 mmol) in toluene (40 ml) was stirred at room temperature for 16 hours. Tris (2-aminoethyl) amine (0.23 g, 1.58 mmol, was added and stirred at 60° C. for 6 hours and cooled then concentrated in vacuo. The reaction mixture was dissolved in toluene, washed with water, dried (MgSO4), filtered and concentrated in vacuo to give the dendrimer as a yellow gum (5.99 g, 97%). ##STR65## cooled The reaction mixture was filtered cooled The reaction mixture was filtered the filtrate was washed with water dried (MgSO4) filtered concentrated in vacuo

反応条件: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: CDI (0.55 g, 3.4 mmol) and KOH (0.1 g, 1.8 mmol) were added to a solution of CIH-HEAP-HEAP-OH (4 g, 3.33 mmol) (as prepared in Example 2(b)) in toluene 50 ml. The reaction mixture was heated to 50-60° C. under nitrogen or 5 hours. Trimethylolpropane (0.15 g, 1.11 mmol) was added and the mixture was stirred for a further 3 hours. The reaction mixture was allowed to cool overnight. The crystallised solid was removed by filtration and the filtrate concentrated in vacuo. The residue was dissolved in dichloromethane, washed with water, dried (MgSO4), filtered and concentrated in vacuo to give the dendrimer product (CIH-HEAP-HEAP-TMP) shown below as a clear viscous liquid (3.96 g, 92%) ##STR54## to cool overnight The crystallised solid was removed by filtration the filtrate concentrated in vacuo The residue was dissolved in dichloromethane washed with water dried (MgSO4) filtered concentrated in vacuo