Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 21111909 | HCID 21111909 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 24755563 | HCID 24755563 | — |
Reaction Steps
4.69 Parts of triphenylsulfonium 4-oxo-1-adamantyloxycarbonyldifluoromethanesulfonate was dissolved in 15 parts of acetonitrile. Into the solution was added dropwise a solution obtained by dissolving 0.15 part of sodium borohydride in 1.51 parts of ion-exchanged water. After the added mixture was stirred for 5 hours, 1N hydrochloric acid was added thereto, and extracted with 1.13 parts of chloroform. After repeatedly washed with ion exchanged water, the organic layer obtained was concentrated. To the concentrate, acetonitrile was added, then the added mixture was concentrated. The concentrate was added dropwise into ethyl acetate. The mixture was filtrated to obtain solid. The solid was dried to obtain 2.20 parts of triphenylsulfonium 4-hydroxy-1-adamantyloxycarbonyldifluoromethanesulfonate in the form of white solid, which is called as acid generator B2. As a result of analyses by 1H-NMR and LCMS, the acid generator B2 determined to be a mixture of two isomers.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08124803B2 |
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| Source dataset | uspto-grants-2012_02 |
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| ORD ID | ord-768717699c4d45b295258e413c343d8a |
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| Source note | uspto-grants-2012_02 |
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