NSC 89798 synthesis
- Product Name:NSC 89798
- CAS Number:83494-25-1
- Molecular formula:C9H7NO3
- Molecular Weight:177.16
65032-27-1
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Yield:-
Reaction Conditions:
in tetrahydrofuran at -40;Inert atmosphere;
Steps:
2.2.1 Preparation of ynols 1a-h
General procedure: To a round bottom flask containing a stirred solution of the aromatic aldehyde (10mmol) in anhydrous THF (20mL) at -40°C and under a dry N2 atmosphere, an ethynyl magnesium chloride solution (10mmol, 6.25mL of a 1.6M solution in THF) was added dropwise. The progress of the reaction was monitored by TLC using n-hexane/ethyl acetate (4:1) as eluent. The reaction mixture was quenched with a saturated solution of NH4Cl (2mL) and the aqueous phase extracted with EtOAc (2×5mL). The organic layer was washed with brine, dried over magnesium sulphate and the solvents removed in a rotatory evaporator. The crude was purified by silica gel chromatography using n-hexane/ethyl acetate (4:1) as eluent, and then concentrated under vacuum for given yields ranging from 75 to 98%.
References:
Silva, Alana B.V.;Silva, Emmanuel D.;dos Santos, Alcindo A.;Princival, Jefferson L. [Catalysis Communications,2020,vol. 137,art. no. 105946]
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4301-14-8
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