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Energy Chemical |
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400-0056266 |
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sales8178@energy-chemical.com |
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| | 2-Bromo-1-(4-morpholinophenyl)-1-ethanone Basic information |
| | 2-Bromo-1-(4-morpholinophenyl)-1-ethanone Chemical Properties |
| Melting point | 112 °C | | storage temp. | Keep Cold | | Sensitive | Lachrymatory |
| Hazard Codes | C | | Risk Statements | 36/37/38-34 | | Safety Statements | 26-36/37/39-45 | | Hazard Note | Corrosive/Lachrymatory/Keep Cold | | HS Code | 2933299090 |
| | 2-Bromo-1-(4-morpholinophenyl)-1-ethanone Usage And Synthesis |
| Synthesis | 1) Preparation of intermediate 4-morpholinophenylacetophenone
Take 50g of 4-fluoroacetophenone, dissolve in 350mL of dimethyl sulfoxide (DMSO) (about 7~8 times the mass volume ratio), stir well, at this time a colorless solution. Slowly add 78.8 g (0.9 mol) of morpholine dropwise at room temperature, dropwise, warm up to 120 reflux. The solution gradually changed to light yellow. The reaction was complete for 3~4h, and the end point of the reaction was monitored by TLC. When the reaction was finished, it was left to room temperature. The reaction solution was slowly poured into a large amount of ice water with stirring, and a yellow solid precipitated. Filter was drawn, the filter cake was collected, washed twice with water and dried to give 63g of yellow solid (85% yield).
(2) Intermediate 2,2-dibromo-1-(4-morpholinophenyl)ethanone preparation
30 g (0.15 mol) of 4-morpholinophenyl ethanone, 210 mL of concentrated sulfuric acid (about 7-8 times the mass to volume ratio), were added to a 500 mL three-necked flask equipped with mechanical stirring and a thermometer and stirred to dissolve. The reaction solution was cooled to 0C, at which temperature 7.8 mL of bromine was slowly dripped in to control the temperature at 0C. After dropping, the reaction was done at room temperature. The reaction was carried out for about 6h and the reaction was monitored for completeness by TLC. The reaction solution was poured into a large amount of ice water and a yellow-green solid precipitated, stirring. After the ice was dissolved, it was filtered and washed with water until neutral. The filter cake was collected and dried to give 47 g of yellow-green solid in 88% yield.
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| | 2-Bromo-1-(4-morpholinophenyl)-1-ethanone Preparation Products And Raw materials |
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