反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
9-(4-Chlorophenyl)-2-(3,4,5-tris(octadecyloxy)-cyclohexylmethoxy)-9-fluorenol (62.0 mg, 51.2 μmol) was dissolved in chloroform (2 mL), acetyl bromide (13 μmol, 172 μmol) was added, and the mixture was stirred at room temperature for 1 hours. After evaporation of the solvent, acetonitrile was added to the residue to allow crystallization to give 9-(4-chlorophenyl)-2-(3,4,5-tris(octadecyloxy)-cyclohexylmethoxy)-9-bromofluorene (63.9 mg, 50.2 μmol, 98%). δ=0.88 (9H, t, J=6.6 Hz, OC18H37 C18-H) 1.1-1.9 (101H, br, Cyclohexyl C1,2,6-H, OC18H37 C2-17-H) 3.16 (2H, d, J=10.3 Hz, Cyclohexyl C3,5-H) 3.46 (4H, m, 3,5-OC18H37 C1-H) 3.68 (2H, t, J=6.7 Hz, 4-OC18H37 C1-H) 3.82 (2H, m, fl-O—CH2—) 3.92 (1H, s, Cyclohexyl C4-H) 6.90 (1H, d, J=8.3 Hz, fl C3-H) 6.96 (1H, s, fl C1-H) 7.18-7.26 (3H, m,Ph C3,5-H, fl C7-H) 7.34 (1H, t, J=7.1 Hz, fl C6-H) 7.43 (1H, d, J=7.6 Hz, fl C8-H) 7.48 (2H, d, J=8.7 Hz, Ph C2,6-H) 7.57 (2H, m, fl C4,5-H)
WORKUP
后处理
- customAfter evaporation of the solvent, acetonitrile
- additionwas added to the residue
- customcrystallization