Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Peracetic Acid | HCID 6585 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 14274523 | HCID 14274523 | — |
| Reactant | HCID 18945546 | HCID 18945546 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14274524 | HCID 14274524 | 98% |
Reaction Steps
To show another example of the epoxy-sulfonylazide of the instant invention, a solution of p-methallyloxybenzenesulfonylazide (506 parts) in methylene chloride (1,450) parts is stirred and heated to reflux (41° C.) then a solution of 35% peracetic acid in acetic acid (521.5 parts) containing sodium acetate (15.6 parts) is added slowly from an addition funnel over 15 minutes. An additional 40 parts of methylene chloride is added to adjust the reflux temperature to 45° C. After 6 hrs stirring and refluxing at 45° C. the reaction is quenched with 835 parts of distilled water. The layers are separated and the organic phase is washed with 555 parts of 10% sodium sulfite, 835 parts of sodium bicarbonate, and 565 parts of distilled water containing 23 parts of trioctylammonium chloride. The solution is dried azeotropically, and the solvent is removed at 55° C. and 20 mm to yield 528 parts of 3-(p-azidosulfonylphenoxy)-2-methylpropylene oxide as a white, crystalline solid. This represents a yield of 98%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04897144 |
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| Source dataset | uspto-grants-1990_01 |
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| ORD ID | ord-79384cb9f8e24d9bb1648c2bb5324b77 |
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| Source note | uspto-grants-1990_01 |
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