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5-BroMo-1-trityl-1H-iMidazole synthesis

2synthesis methods
-

Yield:121816-82-8 75.51%

Reaction Conditions:

with triethylamine in dichloromethane at 0 - 20; for 3 h;

Steps:

116 Synthesis of compound 116.1

To a solution of 5-bromo-lH-imidazole (3.0g, 20.41mmol, l .Oeq) in dichloromethane (30mL) were added triethyl amine (5.833g, 57.76mmol, 2.83eq). Trityl chloride (6.15g, 22.04mmol, 1.08eq) was added dropwise into reaction mixture at 0°C. The reaction mixture was stirred at room temperature for 3h. After completion of reaction, reaction mixture was transferred into water and product was extracted with dichloromethane. Combined organic layer washed with brine solution, dried over sodium sulfate and concentrated under reduced pressure to obtain crude material. This was further triturated with diethyl ether to obtain pure 116.1. (6.0g, 75.51 %). MS(ES): m/z 390.30 [M+H]+.

References:

WO2018/71794,2018,A1 Location in patent:Paragraph 00616; 00617