Hi everyone,
I’m in the process of preparing 500g of 5CL and have the following chemicals on hand:
1. 1H-INDAZOLE-3-CARBOXYLIC ACID METHYL ESTER (CAS 43120-28-1) - 0.5kg
2. N,N-Dimethylformamide (DMF) (CAS 68-12-2) - 1.5kg
3. 5-Bromo-1-pentene (CAS 1119-51-3) - 0.5kg
4. Potassium carbonate (CAS 584-08-7) - 0.5kg
I’m a bit concerned about the process and would really appreciate your advice to ensure everything goes smoothly. Here’s the procedure I’m planning to follow:
**Steep 1:** Dissolve 0.5kg of the main precursor (1H-Indazole-3-Carboxylic Acid Methyl Ester) in 1.5kg of DMF at room temperature until homogeneous.
**Steep 2:** Increase the temperature to 70-80°C (planning to use around 75°C), then add 0.5kg of potassium carbonate to the solution and stir for 2-3 hours.
**Steep 3:** After 2-3 hours, when the potassium carbonate has mostly dissolved, add 0.5kg of 5-Bromo-1-pentene to the mixture. Maintain the temperature and stir for another 2-3 hours.
**Steep 4:** After stirring, cool the solution to room temperature. Slowly pour the mixture into 10L of ice water, stirring quickly to induce crystallization.
**Steep 5:** Filter the solids and rinse with a saturated NaCl solution to remove any water-soluble impurities.
**Steep 6:** Dry the product by hanging in a cool place (25-35°C) or placing it in the refrigerator.
I have a couple of specific questions:
- What should be the appropriate stirring speed (rpm) for each step?
- Can I use a magnetic stirrer instead of an overhead stirrer for this process?
Any insights or suggestions would be greatly appreciated. Thanks in advance for your help!
I’m in the process of preparing 500g of 5CL and have the following chemicals on hand:
1. 1H-INDAZOLE-3-CARBOXYLIC ACID METHYL ESTER (CAS 43120-28-1) - 0.5kg
2. N,N-Dimethylformamide (DMF) (CAS 68-12-2) - 1.5kg
3. 5-Bromo-1-pentene (CAS 1119-51-3) - 0.5kg
4. Potassium carbonate (CAS 584-08-7) - 0.5kg
I’m a bit concerned about the process and would really appreciate your advice to ensure everything goes smoothly. Here’s the procedure I’m planning to follow:
**Steep 1:** Dissolve 0.5kg of the main precursor (1H-Indazole-3-Carboxylic Acid Methyl Ester) in 1.5kg of DMF at room temperature until homogeneous.
**Steep 2:** Increase the temperature to 70-80°C (planning to use around 75°C), then add 0.5kg of potassium carbonate to the solution and stir for 2-3 hours.
**Steep 3:** After 2-3 hours, when the potassium carbonate has mostly dissolved, add 0.5kg of 5-Bromo-1-pentene to the mixture. Maintain the temperature and stir for another 2-3 hours.
**Steep 4:** After stirring, cool the solution to room temperature. Slowly pour the mixture into 10L of ice water, stirring quickly to induce crystallization.
**Steep 5:** Filter the solids and rinse with a saturated NaCl solution to remove any water-soluble impurities.
**Steep 6:** Dry the product by hanging in a cool place (25-35°C) or placing it in the refrigerator.
I have a couple of specific questions:
- What should be the appropriate stirring speed (rpm) for each step?
- Can I use a magnetic stirrer instead of an overhead stirrer for this process?
Any insights or suggestions would be greatly appreciated. Thanks in advance for your help!
