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Type | HazMat fee for 500 gram (Estimated) |
Excepted Quantity | USD 0.00 |
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CAS No. : | 15430-52-1 | MDL No. : | MFCD00012907 |
Formula : | C3H6ClN | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | IKXNIQJDNKPPCH-UHFFFAOYSA-N |
M.W : | 91.54 | Pubchem ID : | 11205720 |
Synonyms : |
|
Signal Word: | Danger | Class: | 6.1 |
Precautionary Statements: | P261-P301+P310-P305+P351+P338 | UN#: | 2811 |
Hazard Statements: | H301-H315-H319-H335 | Packing Group: | Ⅱ |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1.24 g | With sodium hydrogencarbonate; at 20℃;Cooling with ice; | A solution of 1.08 grams of propargylamine hydrochloride in 50 ml of saturated sodium bicarbonate was cooled with an ice water bath, and 2.0 grams of <strong>[55750-49-7]N-carboethoxymaleimide</strong> were added portionwise over a few minutes. The reaction was stirred in the cold for 30 min., then while warming to room temperature over 25 min. The reaction was then extracted with 3*25 ml of dichloromethane, which was dried over sodium sulfate, filtered and concentrated. The residue was taken up in 10 ml of ethyl acetate and heated at 50 C. for two hours to complete the cyclization. The reaction was concentrated and the residue was which was subjected to flash column chromatography on silica gel with 30% ethyl acetate in hexane. A second chromatography as before gave 1.24 g of the product as a very light yellow oil. NMR (CDCl3): delta 6.77 (s, 2H, CHC=O), 4.30 (d, 2H, NCH2, J=2.4 Hz), 2.22 (t, 1H, CCH, J=2.5 Hz). |
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