135235-81-3Relevant articles and documents
Crystal of fumarate of salmeterol intermediate and preparation process thereof
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Paragraph 0036; 0041; 0042; 0043; 0044, (2017/08/28)
The invention discloses a crystal of fumarate of a salmeterol intermediate and a preparation process thereof. The preparation process comprises the following steps: dissolving 6-benzylamino-1-(4'-phenylbutoxy)hexane in alcohol; adding fumaric acid; carrying out heating to 50 to 60 DEG C and carrying out stirring to allow the above substance to be thoroughly dissolved; carrying out cooling to 37 to 40 DEG C within 2 to 4 h so as to allow a crystal to be precipitated, and maintaining the temperature for 2 to 3 h; then allowing the temperature to drop to 12 to 15 DEG C within 6 to 8 h; and successively carrying out ageing for 8 to 12 h, filtering and drying so as to obtain a white solid so as to obtain the fumarate of the salmeterol intermediate 6-benzylamino-1-(4'-phenylbutoxy)hexane. The crystal obtained in the invention has good stability and can be stored for a long time; the preparation process is convenient to operate and easy for industrialization; the alcohol used in the invention is a low-toxicity solvent selected from an organic solvent; and the crystal form of the fumarate of the salmeterol intermediate can be stably obtained.
