Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 67333945 | HCID 67333945 | — |
| Reactant | Sodium phosphate (Na3(PO4)2) | HCID 86630341 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 57694218 | HCID 57694218 | — |
Reaction Steps
Under a nitrogen atmosphere, 3,4-bis(butane-1-sulfonyl)dihydrothiophene and chloroform were placed in a reaction vessel to dissolve 3,4-bis(butane-1-sulfonyl)-dihydrothiophene in chloroform. To the solution, thionyl chloride (3.0 equivalents) was added, followed by heating under reflux for 36 hours. A disodium hydrogenphosphate/sodium dihydrogenphosphate buffer which had been adjusted to pH 7 was added to the reaction mixture to quench the reaction, and the reaction mixture was extracted with ethyl acetate. The organic layer was washed three times with saturated brine, and was dried over anhydrous sodium sulfate. The solvent was distilled off. The resultant crude product was purified through a silica gel column (hexane:ethyl acetate=2:1) to obtain the reaction product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08008425B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-45465ef09fe3476fb5a70a91ed727458 |
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| Source note | uspto-grants-2011_08 |
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