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With potassium carbonate; In isopropyl alcohol; at 80℃; for 2h;
(1) A mixed solution of 20.1 parts of 2-acetylamino-p- cresol, 18.8 parts of potassium carbonate and 90 parts of 2-propanol was heated to 80C and18.3 parts of Butane sultone was added dropwise hereto. After the dropwise addition, the solution was stirred at 80C for 2 hours. After it was cooled to room temperature, 20 parts of water was added and then a solution where 42 parts of 35% hydrochloric acid was diluted with 20 parts of water was added dropwise thereto. It was heated to 80C and stirred for 2.5 hours while distilling some of the solvent away, followed by stirring at 100C for 2 hours. It was cooled to room temperature and then salted out by addition of sodium chloride, and the precipitate was separated by filtration and dried to obtain 22.0 parts of a compound of the following formula (42).
The production method of 2-acetamido-4-methylphenylalkyl ether in Example 5 includesThe following steps:(1) in the reactor by adding o-amino-p-cresol,And acetic acid for acetylation, o-amino-p-cresol and acetic acid molar ratio of 1: 1.6,The temperature of the acetylation reaction was 200 C,Pressure is normal pressure,Preparation of <strong>[6375-17-3]o-acetylamino-p-cresol</strong>;(2) step (1) reaction for about 9 hours, the use of liquid phase for testing,If the detection result is less than 0.1% free amino,The reaction of step (1) is continued; if it is less than or equal to 0.1%Then added in the reactorChloropropane or chlorobutane for alkylation,The temperature of the alkylation reaction is from 80 to 100 C,Pressure is normal pressure to 0.5MPA,To obtain 2-acetamido-4-methylphenylpropyl ether or 2-acetamido-4-methylphenylbutyl ether.
The production method of 2-acetamido-4-methylphenylalkyl ether in Example 6 includesThe following steps:(1) in the reactor by adding o-amino-p-cresol,And acetic acid for acetylation,The molar ratio of o-amino-p-cresol to acetic acid was 1: 1.9,The temperature of the acetylation reaction was 180 C,Pressure is normal pressure,Preparation of <strong>[6375-17-3]o-acetylamino-p-cresol</strong>;(2) step (1) reaction for about 9 hours,Using liquid phase for testing,If the detection result is less than 0.1% free amino,The reaction of step (1) is continued; if it is less than or equal to 0.1%In the reactor by adding methyl bromide, bromoethane,Bromopropane or bromobutane for alkylation,The temperature of the alkylation reaction is from 50 to 95 C,Pressure at atmospheric pressure to 0.2MPa,To give 2-acetamido-4-methylanisole,2-acetamido-4-methylphenylether,2-acetamido-4-methylphenylpropyl ether or 2-acetylamino-4-methylphenylbutyl ether.
In the production of 2-acetamido-4-methylphenylalkyl ether, comprising the steps of:(1) in the reactor by adding o-amino-p-cresol,And acetic acid for acetylation,The molar ratio of o-methyl-p-cresol to acetic acid was 1: 2.5,The temperature of the acetylation reaction was 160 C,Pressure at atmospheric pressure, the preparation of o-acetylamino p-cresol;(2) step (1) reaction for about 9 hours,Using liquid phase for testing,If the detection result is the presence of ammonia ions,The reaction of step (1) is continued;If the reaction result is that there is no ammonia ion,The alkylation reaction is carried out by adding dimethyl sulfate to the reaction kettle,The temperature of the alkylation reaction was 100 C,Pressure is normal pressure,To give 2-acetylamino-4-methylanisole.
In the production of 2-acetamido-4-methylphenylalkyl ether, comprising the steps of:(1) in the reactor by adding o-amino-p-cresol,And acetic acid for acetylation,The molar ratio of o-methyl-p-cresol to acetic acid was 1: 2.5,The temperature of the acetylation reaction was 160 C,Pressure at atmospheric pressure, the preparation of o-acetylamino p-cresol;(2) step (1) reaction for about 9 hours,Using liquid phase for testing,If the detection result is the presence of ammonia ions,The reaction of step (1) is continued;If the reaction result is that there is no ammonia ion,The alkylation reaction is carried out by adding dimethyl sulfate to the reaction kettle,The temperature of the alkylation reaction was 100 C,Pressure is normal pressure,To give 2-acetylamino-4-methylanisole.
The production method of 2-acetamido-4-methylphenylalkyl ether in Example 2 includesThe following steps:(1) in the reactor by adding o-amino-p-cresol,And acetic acid for acetylation,The molar ratio of o-methyl-p-cresol to acetic acid was 1: 2, the temperature of acetylation was 175 ,Pressure is normal pressure,Preparation of <strong>[6375-17-3]o-acetylamino-p-cresol</strong>;(2) step (1) reaction for about 9 hours, the use of liquid phase for testing,If the detection result is less than 0.1% free amino,The reaction of step (1) is continued;If the reaction result is less than or equal to 0.1% of the free amino content,Then added in the reactorMethyl chloride was subjected to methylation reaction,The methylation reaction temperature was 100 C,Pressure of 1MPa,To give 2-acetylamino-4-methylanisole
The production method of 2-acetamido-4-methylphenylalkyl ether in this Example 4 includesThe following steps:(1) in the reactor by adding o-amino-p-cresol, and add acetic acid for acetylation, oThe molar ratio of amino-p-cresol to acetic acid was 1: 1.7, and the temperature of the acetylation reaction was 190 CForce is normal pressure,Preparation of <strong>[6375-17-3]o-acetylamino-p-cresol</strong>;(2) step (1) reaction for about 9 hours,Use liquid to detect, if the test resultsFree amino group greater than 0.1%The reaction of step (1) is continued; if it is less than or equal to 0.1%Then added in the reactorEthyl chloride was subjected to an ethylation reaction,The temperature of the ethylation reaction was 85 C,The pressure is 0.75MPa,To give 2-acetamido-4-methylphenylether
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