Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 15173281 | HCID 15173281 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18417946 | HCID 18417946 | 90% |
Reaction Steps
To a mixture of N-methoxy-N,2,2,5-tetramethyl-1,3-dioxane5-carboxylic acid amid (1.07 g, 4.92 mmol) and THF (10 mL) was gradually added 3 mol/L methylmagnesium bromide in THF (2.46 mL, 7.4 mmol) at 0° C. under nitrogen atmosphere, and the resulting mixture was stirred at 0° C. for 4 hours. After the reaction was completed, saturated ammonium chloride aqueous solution was added to the reaction mixture and the resulting mixture was extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous sodium sulphate, and concentrated in vacuo to give 1-(2,2,5-trimethyl-1,3-dioxane5-yl)ethanone (0.76 g, yield: 90%) as colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08575197B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-71e8852559874cb980b16eb4e98b8d8b |
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| Source note | uspto-grants-2013_11 |
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