Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Triethanolamine | HCID 7618 | — |
| Reactant | 9-(Dicyanomethylidene)-9H-fluorene-4-carbonyl chloride | HCID 19833255 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14438699 | HCID 14438699 | — |
Reaction Steps
A solution of 100.0 grams of triethanolamine and 58 milliliters of dry pyridine in 350 milliliters of dry dichloromethane was stirred at room temperature under a nitrogen atmosphere. A solution of 8.0 grams of (4-chloroformyl-9-fluorenylidene)malononitrile in 400 milliliters of dry dichloromethane was added over a period of 1 hour. After addition, the reaction mixture was further stirred for another hour. The reaction mixture was washed several times with water to remove the excess amines and the corresponding hydrochloride salts, dried with anhydrous magnesium sulfate and filtered. Evaporation of the filtrate gave 5 grams of crude product. Purification by recrystallization from isopropanol afforded 4.5 grams of pure (1c), mp., 155.5°-156.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04835081 |
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| Source dataset | uspto-grants-1989_05 |
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| ORD ID | ord-9b8399d3cc134ac78069fbfb0fbd8d50 |
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| Source note | uspto-grants-1989_05 |
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