Method for synthesizing intermediate N-[2-(2-hydroxyethyl)ethylsulfonyl]-4-nitrobenzenesulfonamide
A technology of nitrobenzenesulfonamide and hydroxyethyl, which is applied in the field of synthesis of intermediate N-[2-ethylsulfonyl]-4-nitrobenzenesulfonamide, can solve the problem of low utilization rate of dyestuff, shortening of reaction time, Problems such as dye intermediate yield resource waste, etc., to achieve the effect of increasing yield and reducing isomerization reaction
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Embodiment 1
[0017] A kind of synthetic method of intermediate N-[2-(2-hydroxyethyl) ethyl sulfone base]-4-nitrobenzenesulfonamide, comprises the following steps:
[0018] Step 1. Dissolve 55.4g of 4-nitrobenzenesulfonyl chloride and 25.3g of 2-amino-2-hydroxyl-diethylsulfide in 200mL of toluene with stirring in an ice-water bath, and add 2.0g of Fe 3 o 4 @TiO 2 The catalyst was magnetically stirred for 3 hours, and the NaOH solution with a concentration of 30% was used to keep the system pH=10, and the reaction was monitored by TLC;
[0019] Step 2. After the stirring is completed, continue to stir and react in an ice bath for 1 hour, and refrigerate overnight in a -4°C refrigerator. After the reaction is completed, adjust the pH of the system to 5 with glacial acetic acid, and add 0.2 g of tungstic acid;
[0020] Step 3. Under the condition of sufficient mechanical stirring at room temperature, slowly add 30ml of 30% hydrogen peroxide dropwise. After 15 minutes of completion of the dro...
Embodiment 2
[0027] Step 1. Dissolve 45.4g of 4-nitrobenzenesulfonyl chloride and 25.3g of 2-amino-2-hydroxyl-diethylsulfide in 200mL of toluene with stirring in an ice-water bath, and add 2.0g of Fe 3 o 4 @TiO 2 The catalyst was magnetically stirred for 3 hours, and the pH of the system was maintained at 10 with a 30% NaOH solution, and the reaction was monitored by TLC; the rest of the steps were the same as in Example 1.
Embodiment 3
[0029] Step 1. Dissolve 35.4g of 4-nitrobenzenesulfonyl chloride and 25.3g of 2-amino-2-hydroxyl-diethylsulfide in 200mL of toluene with stirring in an ice-water bath, and add 2.0g of Fe 3 o 4 @TiO 2 The catalyst was magnetically stirred for 3 hours, and the pH of the system was maintained at 10 with a 30% NaOH solution, and the reaction was monitored by TLC; the rest of the steps were the same as in Example 1.
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