ChemicalBook CAS DataBase List 4-[2-(1-AZEPANYL)ETHOXY]BENZYL CHLORIDE HCL

4-[2-(1-AZEPANYL)ETHOXY]BENZYL CHLORIDE HCL synthesis

8synthesis methods

Product Name:4-[2-(1-AZEPANYL)ETHOXY]BENZYL CHLORIDE HCL
CAS Number:223251-25-0
Molecular formula:C15H23Cl2NO
Molecular Weight:304.26

(4-(2-(azepan-1-yl)ethoxy)phenyl)Methanol

223251-16-9

4-[2-(1-AZEPANYL)ETHOXY]BENZYL CHLORIDE HCL

223251-25-0

S4: (4-(2-(Azepan-1-yl)ethoxy)phenyl)methanol (561 g) obtained from step S3 was dissolved in 1.2 L of tetrahydrofuran and cooled to 0 °C. Thionyl chloride (320 g) was added slowly and dropwise under stirring, keeping the reaction temperature not exceeding 55 °C, and the reaction was gradually warmed up at this temperature for 6 hours. Upon completion of the reaction, about 600 mL of solvent was removed by distillation. To the residue was added 300 mL of ethyl acetate, the mixture was cooled to 0 °C and stirred for 30 minutes. It was subsequently filtered and the solid was washed with 300 mL of ethyl acetate. The resulting solid was dried to give 1-(2-(4-(chloromethyl)phenoxy)ethyl)azepane hydrochloride (619 g) in 90% yield and 99% HPLC purity.

223251-16-9 Synthesis

223251-16-9
39 suppliers
$19.00/250mg

223251-25-0
170 suppliers
$10.00/1g

Yield: 90%

Reaction Conditions:

with thionyl chloride in tetrahydrofuran at 0 - 55; for 6 h;

Steps:

3.4
S4: 561 g of 4- (2-Hexamethyleneimino-1-) ethoxy) Benzyl alcohol obtained from S3 is added into 1.2 liter of tetrahydrofuran, cooled at 0 ° C, added the drops of 320 g of thionyl chloride, after that temperature is gradually raised at 55 ° C for 6 hours, about 600 ml of the solvent is distilled off, 300 ml of ethyl acetate is added to the residue, the mixture is cooled at 0 ° C and stirred for 30 minutes, filtered, washed with 300 ml of ethyl acetate, dry, and then obtained 619 g of 1- (2- (4- (chloro methyl) phenoxyl) ethyl) azacycloheptane hydrochloride, yield 90% and measured HPLC purity 99%.

References:

Jinan Mei Gao Bio-pharmaceutical Technology Co., Ltd.;Xiao Tong;Dong Yuehui;Chen Maoying;Kou Zengjie CN107400087, 2017, A Location in patent:Paragraph 0045