Pyridine → HCID 22630254, compound
Reaction equation
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].[CH2:8]([O:13][C:14]1[CH:26]=[CH:25][C:24]2[C:23]3[C:18](=[CH:19][C:20]([CH2:27][CH2:28][C:29]4[CH:34]=CC(O)=[CH:31][CH:30]=4)=[CH:21][CH:22]=3)[CH2:17][C:16]=2[CH:15]=1)[CH2:9][CH2:10][CH2:11][CH3:12].N1C=CC=CC=1>O>[C:5]([O:4][C:1]1[CH:31]=[CH:30][C:29]([CH2:28][CH2:27][C:20]2[CH:19]=[C:18]3[C:23]([C:24]4[CH:25]=[CH:26][C:14]([O:13][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])=[CH:15][C:16]=4[CH2:17]3)=[CH:22][CH:21]=2)=[CH:34][CH:2]=1)(=[O:7])[CH3:6]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
Acetic anhydride (5 mL) was slowly added to a mixture of 4-(2-(2-pentyloxyfluorene-7-yl)ethyl)phenol (5 g) produced according to the first to ninth steps in Example 1 and pyridine (100 mL) while maintaining 0° C., and the solution was stirred at the same temperature for 2 hours. The reaction mixture was poured into ice and water (200 mL), and the product was extracted with toluene (50 mL). The toluene layer was dried on anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The resulting residue was purified by means of column chromatography (silica gel, eluting solvent: toluene) to obtain 4-(2-(2-pentyloxyfluorene-7-yl)ethyl)phenyl acetate (5.1 g).
Workup
- customproduced
- extractionthe product was extracted with toluene (50 mL)
- dry with materialThe toluene layer was dried on anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe resulting residue was purified by means of column chromatography (silica gel, eluting solvent: toluene)
Sources & evidence
- ORD record
- ord-bfcf9ae7d5b047d3ac0c3a9ae7f6ea2f
- Source dataset
- uspto-grants-2004_11
- Patent number
- US06824709B2
Reaction notes
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