Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Propargyl alcohol | HCID 7859 | — |
| Reactant | 2-Methoxy-2-butene | HCID 111206 | — |
| Catalyst | Phosphoric Acid | HCID 1004 | — |
| Catalyst | Sodium Carbonate | HCID 10340 | — |
| Product | HCID 86668669 | HCID 86668669 | 102.2% |
Reaction Steps
A mixture of 130 mg (0.3 μmol) of phosphoric acid (19% w/w in acetone) and 22.80 g (399 mmol) of propargyl alcohol is filled into a dropping funnel. 53.5 g (598 mmol) of 2-methoxy-but-2-ene (96.2% GC) was transferred into a second dropping funnel. Both solutions were added simultaneously within 30 minutes to the cooled flask (8° C.). The internal temperature was maintained between 8° C. and 12° C. during the addition of the reactants. The reaction mixture was held at 10° C. for about 2 hours. The reaction mixture was neutralized with 0.5 g of sodium carbonate and concentrated under reduced pressure (40° C., 80 mbar). The crude product was analyzed by GC. 58.0 g of crude 2-methoxy-2-prop-2-ynyloxy-butane were obtained with a purity of 85.5% (yield 96.9% based on propargyl alcohol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09045404B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-de66f67235a7402ab111fa9e4e75b17c |
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| Source note | uspto-grants-2015_06 |
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