23460-76-6Relevant articles and documents
-
Allen,Bernstein
, p. 1028,1031 (1955)
-
Synthesis method of triene acetate compound
-
Paragraph 0011-0012; 0017-0018; 0021-0022, (2020/02/10)
The invention belongs to the technical field of steroid hormone preparation, in particular to a synthesis method of a triene acetate compound. The preparation method comprises the following steps: under the participation of 4-dimethylaminopyridine, removing 17-site hydroxyl of the anecortave acetate by using an N-chlorosuccinimide and a sulfur dioxide pyridine solution; and after the reaction is finished, performing crystallization to obtain the triene acetate compound. The 4-dimethylaminopyridine is added into the reaction system, an intermediate is stabilized, generation of rearrangement impurities is well inhibited, and the content of the rearrangement impurities in the system is reduced from 12% to 2%, so that the triene acetate compound is obtained at a high yield, with the purity reaching 99%, and the yield being 80% or above.
Preparation method of delta 16 steroid
-
Paragraph 0082; 0083; 0084; 0085; 0086, (2016/10/07)
The invention relates to a preparation method of a delta 16 steroid. At the atmosphere of protective gas, a compound of a formula II, an oxidizing agent and sulfur dioxide are subjected to a reaction in an organic solvent, the reaction temperature ranges from minus 50 DEG C to 0 DEG C, and the reaction time is 1.5-2.5 h to obtain a delta 16 steroid I, wherein R1 is selected from H, halogen and acyloxy or hydroxide of C1-5; R2 is selected from alkyl of alpha C1-3 and alkyl or H of beta C1-2; R3 is selected from H, alkyl of alpha C1-3, alkyl of beta C1-2, alpha halogen or beta halogen; R4 and R5 are equal to H or double bonds; R7 is selected from H, and R6 is selected from H, alkyl of C1-3 or acyloxy of C1-5; or R6 and R7 are equal to double bonds. According to the preparation method of the delta 16 steroid, the 17-bit hydroxide compound of the formula II is used as raw materials, and the compound of the formula II is industrially produced and is easy to obtain; the preparation method is mild in reaction condition, no high-temperature strong base or strong acid is needed, fewer by-products are produced, the product yield and purity are high, the yield reaches more than 90%, and the purity reaches more than 93%.
