XANTHENE-9-CARBONITRILE synthesis
- Product Name:XANTHENE-9-CARBONITRILE
- CAS Number:85554-24-1
- Molecular formula:C14H9NO
- Molecular Weight:207.23
Yield:85554-24-1 91%
Reaction Conditions:
with potassium iodide in dimethyl sulfoxide at 50 - 80;Solvent;Reagent/catalyst;Concentration;
Steps:
2 9-cyano accounting for tons of synthesis
NaCN (35.3 g, 0.72 mol, 1.2 eq) was dissolved in dry DMSO (80 mL) and potassium iodide (3.0 g,10.0 mmol, 0.03 eq), warmed to 50 ° C, and then 9-chlorohexane (156.7 g, 0.60 mol, 1.0 eq)DMSO (220 mL) was added dropwise for about 1 hour. After the addition was completed, the mixture was heated to 80 ° C. for 8 h. The raw materials for monitoring by TLC were almost disappeared (VPE / EA = 3:2) After the reaction was completed, the mixture was cooled to room temperature, the filtrate was poured into 500 mL of ice water, precipitated solid, filtered, dried at 40 ° C in vacuo,An off-white solid 9-cyano accounted 113g, yield 91%.
References:
CN107353275,2017,A Location in patent:Paragraph 0035; 0040; 0041; 0044; 0049; 0050
5813-90-1
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90-46-0
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