ChemicalBook CAS DataBase List 6,6'-BIS(CHLOROMETHYL)-2,2'-BIPYRIDINE

6,6'-BIS(CHLOROMETHYL)-2,2'-BIPYRIDINE synthesis

12synthesis methods

Product Name:6,6'-BIS(CHLOROMETHYL)-2,2'-BIPYRIDINE
CAS Number:74065-64-8
Molecular formula:C12H10Cl2N2
Molecular Weight:253.13

74065-63-7 Synthesis

74065-63-7
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74065-64-8
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Yield:74065-64-8 90%

Reaction Conditions:

with thionyl chloride in dichloromethane at 0 - 45; for 3.25 h;Inert atmosphere;Schlenk technique;

Steps:

3 6,6'-dichloromethyl-2,2'-bipyridine (17)

In a dry and clean dish with a tandem and a magnetic stirrer100 mL of a Schlenk flask was added 16 (1.71 g, 7.91 mmol). The system was replaced with argon atmosphere and anhydrous dichloromethane (40 mL) was added. The system was incubated at 0 ° C with an ice salt bath and dropped onto the system by syringe DripThionyl chloride (4.81 g, 40.4 mmol) was diluted in dichloromethane(10 mL) was added dropwise over a period of 15 minutes.Drop finished, remove the cold bath, heated to 45 with oil bath stirring reaction 3 hours,TLC was monitored. The system was cooled to room temperature and poured into a beaker containing ice (100 g). The mixture was triturated with 6N NaOH aqueous solution (pH = 13) and extracted with dichloromethane (3 x 50 mL) Followed by water (100 mL) and saturatedAnd brine (100 mL), dried over anhydrous sodium sulfate and allowed to stand. The desiccant was removed by suction filtration, and the filtrate was desolved with a rotary evaporator,A light yellow solid product, 1.80 g, was obtained in a yield of 90%.

References:

CN103980317,2017,B Location in patent:Paragraph 0062; 0064

49669-26-3 Synthesis