Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | HCID 86753072 | HCID 86753072 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86753073 | HCID 86753073 | 74.9% |
Reaction Steps
3.10 g of trifluoromethanesulphonic anhydride dissolved in 10 ml of dichloromethane was added dropwise at 0° C. to a solution of 4.40 g of 4-[2',3'-difluoro-4"-(4-hydroxy-butyl)-1,2':4',1"-terphenyl-4-yloxy]-butyl acrylate and 1.18 g of lutidine in 100 ml of dichloromethane. The reaction mixture was stirred at 0° C. for 90 minutes and subsequently poured into 100 ml of water and extracted twice with 50 ml of dichloromethane. The combined organic phases were washed twice with 50 ml of water each time, dried over magnesium sulphate and concentrated. Chromatographic purification of the residue on silica gel with cyclohexane/ethyl acetate (vol. 8:2) gave 4.20 g of 4-[2',3'-difluoro-4"-[4-(trifluoro-methanesulphonyloxy)-butyl]-1,2':4',1"-terphenyl-4-yloxy]-butyl acrylate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05800733 |
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| Source dataset | uspto-grants-1998_09 |
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| ORD ID | ord-08d2e2b4f3cd442fb5d19b2fb93a26d7 |
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| Source note | uspto-grants-1998_09 |
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