Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phosphine | HCID 24404 | — |
| Reactant | HCID 18676581 | HCID 18676581 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 18676583 | HCID 18676583 | — |
Reaction Steps
2.1 g (4.4 mmol) of 2,6-bis(2,4,5-trimethylphenyl)-4-phenylpyrylium tetrafluoroborate in 150 ml of n-butanol were used as starting material. The autoclave product obtained after the reaction with PH3 was evaporated to about 50 ml under reduced pressure at about 80° C. The solid which precipitated was filtered off with suction, washed with n-pentane and subsequently dissolved in toluene. The toluene solution was then washed with water until the aqueous phase was neutral. After removing the solvent and washing with a little n-pentane, the residue was dissolved in dichloromethane. The resulting solution was diluted with methanol and then evaporated under reduced pressure at 30° C. until a solid precipitated. The solid was filtered off with suction, washed with a little n-pentane and subsequently dried in a high vacuum. Yield: 0.8 g (45%) of light-yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06509505B1 |
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| Source dataset | uspto-grants-2003_01 |
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| ORD ID | ord-b95821438ba84824b9b5114f2a7a6de0 |
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| Source note | uspto-grants-2003_01 |
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