Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 86594131 | HCID 86594131 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59853915 | HCID 59853915 | — |
Reaction Steps
375 mg (1.00 mmol) of 2-[4-(5H-dibenzo[a,d][7]annulen-5-ylidene)-1-piperidinyl-2-oxoethanamine hydrochloride was dissolved in 3 ml of dichloromethane. 303 mg (3.00 mmol) of triethylamine was added to the obtained solution. Then a solution of 130 mg (1.20 mmol) of ethyl chloroformate in 3 ml of dichloromethane was slowly added to the reaction mixture. After stirring overnight, saturated aqueous sodium hydrogencarbonate solution was added thereto. After extracting with ethyl acetate twice followed by drying under anhydrous sodium sulfate, the solvent was evaporated under reduced pressure. The residue was roughly purified by the silica gel chromatography (dichloromethane: methanol=98: 2) and then purified by the silica gel chromatography (hexane:ethyl acetate=1:2) to obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07713957B2 |
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| Source dataset | uspto-grants-2010_05 |
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| ORD ID | ord-6bc17da1935447838bcf11beb339b40d |
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| Source note | uspto-grants-2010_05 |
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