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CAS No. : | 18355-96-9 | MDL No. : | MFCD00012200 |
Formula : | C23H27BrNP | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | SSWPSKSQQSJKKF-UHFFFAOYSA-M |
M.W : | 428.35 | Pubchem ID : | 15982517 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
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 |
---|---|---|
60.6% | (1) Add 200g (3-dimethylaminopropyl)triphenylphosphine bromide to the three-necked flask, and then add 400g of anhydrous tetrahydrofuran, turn on the stirring, and control the temperature to 20-22 C.After adding 40 g of NaH, the temperature was raised to reflux after the addition, and the reaction was carried out for 1 h.Then add 100g of isoc acid, stir under reflux for 2 hours, then lower the temperature to 0 ~ 15 , slowly add 30g of anhydrous methanol,Then, 400 g of a 50% mass concentration tetrahydrofuran aqueous solution was added, and finally 1600 g of water was added to quench the reaction.The reaction solution was adjusted to pH 6 ± 0.2 with concentrated hydrochloric acid, and then distilled to dryness under reduced pressure.The solid was dissolved in 1400 g of acetone, stirring was started, 40 g of concentrated hydrochloric acid was added, and a white solid was precipitated.After the dropwise addition was completed, the temperature was lowered to 10 to 15 C and stirred for another 10 hours.Suction filtration to obtain a white solid, dried in an oven to constant weight. The product was crude olopatadine hydrochloride,The purity is 98.67% (Z / E = 98.67: 0.82), the yield is 62.4g, and the yield in this step is 60.6%. |