Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 20460154 | HCID 20460154 | — |
| Reactant | HCID 54343097 | HCID 54343097 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 54270134 | HCID 54270134 | — |
Reaction Steps
1-Hydroxy-3,7-dimethylfluoren-9-one (0.01 mole), triethylamine (0.011 mole) and toluene (75 ml) are charged into a glass reaction flask equipped with a stirrer, thermometer and addition funnel. The mixture is cooled to about -10° C. and a solution of O-(2-methyl-4-chlorophenyl) methylphosphonochloridate (0.011 mole) in toluene (25 ml) is slowly added with stirring. After the addition is completed the reaction mixture is allowed to slowly warm to room temperature and stirring is continued for a period of 24 hours. After this time the reaction mixture is filtered and the filtrate is stripped of solvent leaving a residue. This residue is subjected to column chromatography using mixtures of ethyl acetate and hexane as the eluant. The fractions containing product are combined and stripped of solvent to yield the desired product O-(2-methyl-4-chlorophenyl) O-(3,7-dimethylfluoren-9-one-1-yl) methylphosphonate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04447420 |
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| Source dataset | uspto-grants-1984_05 |
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| ORD ID | ord-473cea0c4fc14914a2357e8fd610834a |
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| Source note | uspto-grants-1984_05 |
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