7-CHLORO-1,2,3,4-TETRAHYDRO-BENZO[B]AZEPIN-5-ONE For Tolvaptan CAS 160129-45-3

Payment Type: L/C,T/T
Incoterm: FOB
Min. Order: 1 Kilogram
Delivery Time: 15 Days

Basic Info

Model No.: 160129-45-3

Additional Info

Packaging: AS REQUIRED

Productivity: KGS

Brand: VOLSENCHEM

Transportation: Air

Place of Origin: CHINA

Supply Ability: TRUE MANUFACTURER

Certificate: ISO

Product Description

The intermediate of tolvaptan 3 CAS number 160129-45-3,7-CHLORO-1,2,3,4-TETRAHYDRO-BENZO[B]AZEPIN-5-ONE which is a key intermediate of tolvaptan, has been reported in many literatures about his synthesis. One of the methods of synthesis has aroused our interest. The general process is like this :use 4-Chloroaniline as raw material, first condensate with p-toluenesulfonyl chloride to protect the amino, and then coupled with 4-bromobutyrate ethyl ester, the resulting product was hydrolyzed, acyl chloride, deprotected ring, and then through six Step reaction to obtain the target product tolvaptan intermediate 3 CAS160129-45-3. The yield of the product obtained by the method has great fluctuation and strong instability. There is an improved method to achieve more stable production, the specific steps are as follows: (1), mixing amino chlorobenzene, acid binding agent and aprotic organic solvent, adding 4-chlorobutyric acid Methyl ester and heating to 40-50 ° C,Keep the temperature for 3 to 8 hours to obtain methyl 4 - ((4-chlorophenyl) amino) butanoate; (2) mixing 4 - ((4-chlorophenyl) Amino) butanoate and water. Dropwise inorganic acid at 10-20 ° C, the mixture is heated to 90-100 ° C, reacted for 2-5 hours, then cooled to 0-15 ° C, extracted and concentrated to obtain 4 - ((4- Chlorophenyl) amino) butanoic acid;(3)The mixture of 4 - ((4-chlorophenyl) amino) butanoic acid and thionyl chloride was heated to 40-50 ° C. for 4 hours, concentrated to remove thionyl chloride, and added with methylene chloride solvent to cool down to -5~ 5 ° C, sulfuric acid was added to maintain the system at a pH of 2.0-3.0, Lewis acid was dropwise, keep thermal insulation reaction for 2-3 hours, added alkali solution stirred for 2-3 hours, after standing stratified and concentrated to remove methylene chloride, crystallization , To obtain the target product tolvaptan intermediate 3 CAS160129-45-3.

Thera. Category:  Vasopressin Receptor

Cas No.: 160129-45-3

Synonym:7-chloro-2,3,4,5-tetrahydro-1H-1-benzazepin-5-one;7-Chloro-1,2,3,4-tetrahydro-5H-1-benzazepin-5-one;7-chloro-1,2,3,4-tetrahydro-5H-benzo[b]azepin-5-one;7-CHLORO-1,2,3,4-TETRAHYDRO-BENZO[B]AZEPIN-5-ONE;7-chloro-1, 2, 3, 4-benzo [b] AZA Zhuo-5-ketone;7-Chloro-1,2,3,4-tetrahydro-5H-1-benzozepin-5-one;5H-1-Benzazepin-5-one,7-chloro-1,2,3,4-tetrahydro-;7-Chlorobenzo[b]azepan-5-one;

160129-45-3

Molecular Weight: 195.65

Molecular formula: C10H10ClNO

Assay: ≥98.%

Appearance: White Crystalline solid

Packing:Export worthy packing

Material Safety Data Sheet:Available on request

 

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