7,8-Dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one synthesis
- Product Name:7,8-Dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one
- CAS Number:73942-87-7
- Molecular formula:C12H13NO3
- Molecular Weight:219.24
2.Stir the mixture for 17 hours at 25°C.
3.Monitor the reaction by HPLC (starting material should be less than 4.0%).
4.Pour the reaction mixture on 3.0 kg of crushed ice, if HPLC complies.
5.Stir the mixture for 30 minutes and filter the solid material.
6.Wash the mixture with 1 L of water, suck dry and unload the material.
7.Dry the 7,8-Dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one under vacuum at 55-60°C till the LOD comes to below 0.5%.
73954-34-4
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73942-87-7
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Yield:73942-87-7 77.5%
Reaction Conditions:
with hydrogenchloride;acetic acid in water at 25; for 17 h;
Steps:
8
Example 8Charge 142.0 g of N-(2,2-dimethoxyethyl)- 2-(3,4-dimethoxyphenyl) acetamide (VIII), 710 ml of glacial acetic acid and 710 ml of cone, hydrochloric acid in a 3.0 L RB flask equipped with mechanical stirrer and thermometer pocket at 25°C. Stir for 17 hours at 25°C. Monitor the reaction by HPLC (Compound VIII should be less than 4.0%). If HPLC complies, pour the reaction mixture on 3.0 kg of crushed ice. Stir for 30 minutes and filter the solid material. Wash with 1 L of water, suck dry and unload the material. Dry the material (IX) under vacuum at 55-60°C till the LOD comes to below 0.5%.Weight: 51.0 g Yield: 77.5% HPLC purity: 98.9%
References:
KRKA, D. D., NOVO MESTO;BOSE, Prosenjit;SIRIPALLI, Udaya Bhaskara Rao;KANDADAI, Appan Srinivas WO2010/72409, 2010, A1 Location in patent:Page/Page column 17-18
93-40-3
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73942-87-7
313 suppliers
$23.00/1g
10313-60-7
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73942-87-7
313 suppliers
$23.00/1g
85175-49-1
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73942-87-7
313 suppliers
$23.00/1g