Abstract

3211 under the condition of a reducing agent; (2) directly adding, without separation, a product obtained from step (1) into alkyne as shown in formula I to perform reaction; and (3) directly adding, without separation, a product obtained from step (2) into an olefin as shown in formula II to perform reaction, thereby obtaining a ruthenium carbene compound as shown in formula III. Gaseous explosive ethylene or acetylene gas is prevented from being applied or generated in a process route; a reaction condition is mild, an extremely low temperature or a high temperature is not required; and an operation is simple. Compared with existing routes, the process has stronger operability and economic advantages.

IPC Classes  ?

• C07F 15/00 - Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
• B01J 31/24 - Phosphines
• B01J 31/22 - Organic complexes

Abstract

Disclosed is a highly efficient contrast agent synthesizing method, comprising the following steps: (I) preparing an intermediate mixture of a compound represented by formula (II) and a compound represented by formula (I) and/or formula (III); (II) performing separation to obtain the compound represented by formula (II) and the compound represented by formula (I) and/or formula (III); (III) taking the compound represented by formula (II) to prepare a contrast agent iopromid; and (IV) taking the compound represented by formula (III) to prepare a contrast agent iobitridol; and/or taking a compound represented by formula (I) to prepare a contrast agent iohexol, ioversol, iopentol, or iodixanol. According to the method, by synthesizing and separating intermediates of the compound represented by formula (II) as well as the compound represented by formula (I) and/or formula (III), and then separately preparing contrast agents using the intermediates as the raw materials, the problem of the need to remove a diacylated byproduct in an existing method is overcome, and all intermediates are effectively utilized, the efficiency is high, and the actual application prospect is good.

IPC Classes  ?

• C07C 237/46 - Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups having the carbon atom of at least one of the carboxamide groups bound to a carbon atom of a non-condensed six-membered aromatic ring of the carbon skeleton having carbon atoms of carboxamide groups, amino groups and at least three atoms of bromine or iodine, bound to carbon atoms of the same non-condensed six-membered aromatic ring
• C07C 231/02 - Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines

Abstract

Disclosed is a preparation method for a compound shown by formula (E), a Velpatasvir intermediate shown by formula (K) and an analogue thereof. The method of the present invention uses inexpensive and easily available materials, and a simple process operation, without the need for separating the intermediates, the products are by column chromatography, and it is suitable for industrialized large-scale production..

IPC Classes  ?

• C07C 221/00 - Preparation of compounds containing amino groups and doubly-bound oxygen atoms bound to the same carbon skeleton
• C07C 225/22 - Compounds containing amino groups and doubly-bound oxygen atoms bound to the same carbon skeleton, at least one of the doubly-bound oxygen atoms not being part of a —CHO group, e.g. amino ketones having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton
• C07D 311/78 - Ring systems having three or more relevant rings