5,5'-Dimethyldipyrromethane synthesis

5synthesis methods

Product Name:5,5'-Dimethyldipyrromethane
CAS Number:99840-54-7
Molecular formula:C11H14N2
Molecular Weight:174.24

109-97-7 Synthesis

109-97-7
338 suppliers
$9.00/5G

67-64-1
6 suppliers
$21.60/10ml

99840-54-7
22 suppliers
$110.00/100mg

Yield:99840-54-7 95%

Reaction Conditions:

with trifluoroacetic acid in lithium hydroxide monohydrate at 25; for 0.5 h;

Steps:

1

In a dried 250 mL round-bottom flask, add 100 mL of distilled water as the solvent, add acetone (1.46 mL, 20 mmol) and resteam pyrrole I_a(2.78mL, 40mmol), followed by slow dropwise addition of trifluoroacetic acid (0.20mL, 2.69mmol), the reaction was stirred at 25 °C for 30 minutes, the reaction solution changed from colorless turbidity to milky white turbidity solution, and thin chromatography monitored (petroleum ether: ethyl acetate = 10:1) reaction progress. After the reaction is complete, the reaction solution is poured into the dispensing funnel, the static dispensing is dispensed for 10 minutes, the milky white liquid sinks to the bottom, the upper layer of colorless aqueous solution is poured off, the remaining solution is extracted with ethyl acetate (30mL×2). The organic phase was washed, dried, filtered, and collected with saturated sodium bicarbonate solution (40 mL×3) and saturated saline solution (40 mL×1), respectively. With a rotary evaporator, the solvent ethyl acetate is evaporated to give a yellow liquid, and the crude product is dried on the column, and the separation and purification (petroleum ether: ethyl acetate = 15:1) is separated and purified by 100-200 mesh silica gel chromatography, to obtain compound I_bwhite solid (3.31g, yield of 95%).

References:

CN115043862,2022,A Location in patent:Paragraph 0026-0029

109-97-7 Synthesis

109-97-7
338 suppliers
$9.00/5G

67-64-1
6 suppliers
$21.60/10ml

99840-54-7
22 suppliers
$110.00/100mg