(1,4-diazabicyclo[2.2.2]octan-2-yl)methanol synthesis
- Product Name:(1,4-diazabicyclo[2.2.2]octan-2-yl)methanol
- CAS Number:76950-43-1
- Molecular formula:C7H14N2O
- Molecular Weight:142.2
Yield:76950-43-1 98%
Reaction Conditions:
with N-benzyl-N,N,N-triethylammonium chloride;sodium hydroxide in water at 90 - 95; for 8 h;
Steps:
1 Synthesis Example 1:
The pyridazine and 2,3-dibromopropanol are in a specific ratio(molar ratio 2: 2.1) placed with a stirrer,1 liter four-necked round bottom flask with thermometer and reflux condenser,Add 400 ml of water, 30% of 4 mol of sodium hydroxide,1% by weight of the reactants of benzyltriethylammonium chloride,The temperature was raised to 90-95 ° C for 8 hours.Then, all the water was distilled off, cooled, and then 400 ml of methanol was added thereto, and the mixture was thoroughly stirred, and the by-product sodium bromide was filtered off, and the cake was washed with methanol.The filtrates are combined, concentrated, cooled, crystallized, filtered, dried.The product was obtained in an amount of 135 g, a melting point of 103.2-113.5 ° C, and a GC analysis content of 98% or more.Methanol can be recycled.
References:
CN109096280,2018,A Location in patent:Paragraph 0021; 0022
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