Toluene → 2,6-Dimethyl-4-heptanol

Temperature

60 °C

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##

1. temperaturecooled
2. filtrationThe reaction mixture was filtered
3. temperaturecooled
4. filtrationThe reaction mixture was filtered
5. washthe filtrate was washed with water
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo

ORD record

ord-5e850e6a53b84634998e65fabea9929b

Source dataset

uspto-grants-2000_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06037444