Preparation process of duloxetine
A preparation process and technology of duloxetine, applied in the field of chemical drug preparation, can solve the problems of complexity, incomplete hydrolysis, influence on the purity of duloxetine, etc., and achieve high production safety, guaranteed purity and high reaction yield. Effect
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Embodiment 1
[0020] The present invention proposes a preparation process of duloxetine, comprising the steps of:
[0021] S1: select thiophene, 2-acetylthiophene, 3-chloropropionyl chloride and 1-fluoronaphthalene as raw materials;
[0022] S2: Put thiophene and 2-acetylthiophene in the reactor, raise the temperature in the reactor to 70 degrees Celsius, mix them evenly and stir them, then add 3-chloropropionyl chloride, and Under the effect of reaction, generate 3-chloro-1-(2-thiophene)-acetone;
[0023] S3: Place the 3-chloro-1-(2-thiophene)-acetone in S2 in an environment of 60 degrees Celsius, and slowly add sodium borohydride to it, and mix and stir in real time during the addition, so as to obtain 3- Chloro-1-(2-thiophene)-propanol;
[0024] S4: After the above is completed, add the mixed solution to 3-chloro-1-(2-thiophene)-propanol again, and stir at 100 degrees Celsius for 10 minutes to generate a mixture A;
[0025] S5: Pass 1-fluoronaphthalene into the mixture A, lower the te...
Embodiment 2
[0033] The present invention proposes a preparation process of duloxetine, comprising the steps of:
[0034] S1: select thiophene, 2-acetylthiophene, 3-chloropropionyl chloride and 1-fluoronaphthalene as raw materials;
[0035] S2: Put thiophene and 2-acetylthiophene in the reactor, raise the temperature in the reactor to 75 degrees Celsius, mix them evenly and stir them, then add 3-chloropropionyl chloride, and Under the effect of reaction, generate 3-chloro-1-(2-thiophene)-acetone;
[0036] S3: Place the 3-chloro-1-(2-thiophene)-acetone in S2 in an environment of 70 degrees Celsius, and slowly add sodium borohydride to it, and mix and stir in real time during the addition, so as to obtain 3- Chloro-1-(2-thiophene)-propanol;
[0037] S4: After the above is completed, add the mixed solution to 3-chloro-1-(2-thiophene)-propanol again, and stir at 105 degrees Celsius for 13 minutes to generate a mixture A;
[0038] S5: Pass 1-fluoronaphthalene into the mixture A, lower the te...
Embodiment 3
[0046] The present invention proposes a preparation process of duloxetine, comprising the steps of:
[0047] S1: select thiophene, 2-acetylthiophene, 3-chloropropionyl chloride and 1-fluoronaphthalene as raw materials;
[0048] S2: Put thiophene and 2-acetylthiophene in the reactor, raise the temperature in the reactor to 80 degrees Celsius, mix them evenly and stir them, then add 3-chloropropionyl chloride, and Under the effect of reaction, generate 3-chloro-1-(2-thiophene)-acetone;
[0049] S3: Place the 3-chloro-1-(2-thiophene)-acetone in S2 at an environment of 80 degrees Celsius, and slowly add sodium borohydride to it, and mix and stir in real time during the addition, thereby obtaining 3- Chloro-1-(2-thiophene)-propanol;
[0050] S4: After the above is completed, add the mixed solution to 3-chloro-1-(2-thiophene)-propanol again, and stir at 110 degrees Celsius for 16 minutes to generate a mixture A;
[0051] S5: Pass 1-fluoronaphthalene into the mixture A, lower the ...
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