反应详情

[In analogy to a procedure by Wheeler et. al., J. Am. Chem. Sec. 106, 7404 (1984)] 3.3 g (9.5 mmol) of dimethyl-octadecyl-chlorosilane and 0.5 g (0.8 mmol) of dihydroxygermanium-phthalocyanine in 50 ml of pyridine are stirred for 2 hours at 50°. The solution is cooled and filtered using a suction filter. The solvent is removed in vacuo, and 250 ml of hexane are added to the residue. The resulting precipitate is filtered off with suction and washed first with hexane, then in portions with 200 ml of acetone/water (1:1). The residue is dried overnight under a high vacuum, then extracted with toluene in a Soxhlet, freed of solvent and dried, yielding bis(dimethyl-octadecyl-siloxy)germanium-phthalocyanine; NMR (pyridine-d5): δ=9.8-9.9 (m, 8H); 8.3-8.5 (m,8H): aromatic H's; 0.75-1.46 (various m's); 0.45(m); -0.03 (m); -0.88 (m); -1.91 (m); -2.48 (m, 4×CH3 : silyl side chains) ppm.

1. temperatureThe solution is cooled
2. filtrationfiltered
3. filtrationfilter
4. customThe solvent is removed in vacuo, and 250 ml of hexane
5. additionare added to the residue
6. filtrationThe resulting precipitate is filtered off with suction
7. washwashed first with hexane
8. customThe residue is dried overnight under a high vacuum
9. extractionextracted with toluene in a Soxhlet
10. customdried