Method for preparing 2-methanesulfonyl amino diphenyl ether
A technology of methanesulfonylaminodiphenyl ether and aminodiphenyl ether, which is applied in the field of preparation of 2-methanesulfonylaminodiphenyl ether, can solve the problems of three wastes that are difficult to handle, high toxicity, and long time consumption, and achieve mild reaction, Simple operation and low pollution effect
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Embodiment 1
[0022] (1) Add 185.2g (ie 1.0mol) of o-aminodiphenyl ether and 316g (ie 4.0mol) of pyridine into a reaction flask equipped with stirring, constant pressure dropping funnel and reflux condenser, start stirring, and place in an ice bath Cool down to 0°C;
[0023] (2) Take a beaker and dissolve 191.6g (that is, 1.1mol) methanesulfonic anhydride in 600ml of dichloromethane, then add it to the constant pressure dropping funnel, start to add dropwise, keep the temperature at 0~5℃, and then The dripping is completed within 0.5~1 hour, and then the temperature is kept below 10°C for 4 hours;
[0024] (3) After the reaction is over, pour the reaction solution prepared in step (2) into 800 ml of 18% hydrochloric acid at a temperature of 0 to 5°C, filter, wash the filter cake with water, and dry to obtain 237.0 g of 2-formazan Sulfonylaminodiphenyl ether, the yield is 90%, and the melting point mp is 118~120℃.
[0025] Using hydrogen NMR spectroscopy (H 1 -NMR) to analyze the sample, ...
Embodiment 2
[0031] (1) Add 185.2g (i.e. 1.0mol) o-aminodiphenyl ether and 79.1g (i.e. 1.0mol) pyridine to a reaction flask equipped with stirring, constant pressure dropping funnel and reflux condenser, start stirring, and place on ice Cool in the bath to 0°C;
[0032] (2) Take a beaker and dissolve 348.4g (ie 2mol) of methanesulfonic anhydride in 1100ml of dichloromethane, then add it to the constant pressure dropping funnel, start to add dropwise, keep the temperature at 0~5℃, at 0.5 The dripping is completed within ~1 hour, and then the reaction is kept at below 10°C for 6 hours;
[0033] (3) After the reaction, pour the reaction solution prepared in step (2) into 800 ml of 18% hydrochloric acid at a temperature of 0-5°C, filter, wash the filter cake with water, and dry to obtain 219 g of 2-methanesulfonate Amidodiphenyl ether, the yield is 83.3%, and the melting point mp is 117~120℃.
[0034] Using hydrogen NMR spectroscopy (H 1 -NMR) to analyze the sample, wherein the solvent is d...
Embodiment 3
[0040] (1) Add 185.2g (i.e. 1.0mol) o-aminodiphenyl ether and 474.6g (i.e. 6.0mol) pyridine to the reaction flask equipped with stirring, constant pressure dropping funnel and reflux condenser, start stirring, and place on ice Cool in the bath to 0°C;
[0041] (2) Take a beaker and dissolve 191.6g (that is, 1.1mol) methanesulfonic anhydride in 600ml of dichloromethane, then add it to the constant pressure dropping funnel, start to add dropwise, keep the temperature at 0~5℃, and then Dropping is completed within 0.5~1 hour, and then kept at 10°C for 8 hours;
[0042] (3) After the reaction is over, pour the solution prepared in the reverse step (2) into 800 ml of 18% hydrochloric acid at a temperature of 0 to 5°C, filter, wash the filter cake with water, and dry to obtain 234.9 g of 2- Methylsulfonylaminodiphenyl ether, the yield is 89.3%, and the melting point mp is 118~120℃.
[0043] Using hydrogen NMR spectroscopy (H 1 -NMR) to analyze the sample, wherein the solvent is d...
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