Novel method for synthesizing indole-3-carbinol
A new method, the technology of indole, applied in the field of chemistry, can solve the problems of high cost and excessive benzene residues, and achieve the effects of low equipment corrosion, good thermal stability and good reuse performance.
Inactive Publication Date: 2012-11-07
XIAN UNION PHARMPRO
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Problems solved by technology
[0003] The disadvantage of the existing technology is that the benzene residue exceeds the standard, and the cost of using toluene as a solvent is relatively high
Method used
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Experimental program
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Embodiment Construction
[0014] The method of the present invention will be further described in detail below in conjunction with specific examples.
[0015] A new method for synthesizing indole 3 carbinol, comprising the following steps:
[0016] 1) Accurately weigh 0.2 mol of indole-3 formaldehyde, 200 ml of 99% ethanol, 0.2 mol of potassium borohydride, and react at room temperature for 3 hours;
[0017] 2) decompress to -0.8mpa, concentrate;
[0018] 3) Add 500 ml of water to precipitate a solid, which is the crude product of indole-3methanol.
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The invention provides a novel method for synthesizing indole-3-carbinol. The new method comprises the following steps: 1, accurately preparing 0.2mol of indole-3-formaldehyde, 200ml of ethanol with concentration being 99% and 0.2mol of potassium borohydride and reacting at a room temperature for 3h; 2, reducing pressure to minus 0.8mpa and concentrating; and adding 500ml of water and separating out a solid product which is the crude product of indole-3-carbinol. According to the new method, since medicinal alcohol is used as a solvent, the problem benzene residues exceed the standard is solved and the cost is reduced.
Description
technical field [0001] The invention belongs to the technical field of chemistry and relates to a new method for synthesizing indole-3 carbinol. Background technique [0002] The current industrial synthesis process is to synthesize indole-3-carboxaldehyde according to the Vilsmeier (Vilsmeier.A.) reaction, and then reduce it to indole-3-carbinol. The Vilsmeier reaction is widely used as a formylation method for aromatic compounds (substituted aromatic hydrocarbons, aromatic amines, phenols and phenol ethers, etc.) and heterocyclic compounds (pyrrole, indole, pyridine, etc.). The substituted formamide (DMF or MFA), aromatic and heterocyclic compounds are condensed in the presence of POCl3, and the intermediates formed by condensation are hydrolyzed into corresponding aldehydes in acid solution. When reducing indole-3-carboxaldehyde, toluene is used Aqueous potassium borohydride reduction system. [0003] The disadvantage of the prior art is that the benzene residue exceeds...
Claims
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Inventor 王强陈曦
Owner XIAN UNION PHARMPRO