Processes for the preparation of enamines
A technology of mixtures and reaction zones, used in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc.
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[0120] The examples are for illustrative purposes only, and should not be construed as limiting the present invention disclosed in this document to only the embodiments disclosed in these examples.
[0121] 1. Preparation of 3-methylthiobutyraldehyde from crotonaldehyde (1).
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[0123] A three-liter (L) 3-neck round bottom flask equipped with magnetic stirring, temperature probe, addition funnel, distillation head, protected with nitrogen, and discharged to the bleach scrubber was charged with 100 mL of toluene, and then charged with 84 g (1.39 mol ) Glacial acetic acid, and then filled with 61g (0.86mol) crotonaldehyde. Another 100 mL of toluene was used as a solvent wash during the addition of acetic acid and crotonaldehyde. The reaction mixture was cooled in an ice-water bath, and then 500 g (0.906 mol) of 12.7% by weight sodium methyl mercaptan aqueous solution was added via an addition funnel over 67 minutes (min). During the addition of the thiolate solution, the int...
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