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ChemicalBook CAS DataBase List Iodoform
75-47-8

Iodoform synthesis

14synthesis methods
-

Yield:2782-40-3 85% ,75-47-8 30%

Reaction Conditions:

with tert.-butylhydroperoxide;iodine in water;Petroleum ether at 0; for 12 h;Reagent/catalyst;Solvent;

Steps:

General procedures for amides 3
General procedure: Methyl ketones (0.5mmol), ammines (2.0mmol), I2 (0.55mmol, 110mol%), TBHP (6.0equiv, 70% aqueous solution 401 uL), and 2.0mL of PE, were added to a tube under air. The reaction mixture was stirred at 0°C for 12h. The reaction mixture was quenched with saturated Na2S2O3 solution, extracted repeatedly with ethyl acetate, dried over Na2SO4. It was then removal of the organic solvent in vacuum and followed by flash silica gel column chromatographic purification afforded product with Petroleum/Ethyl acetate mixtures.

References:

Zhu, Chunyin;Wei, Wei;Du, Peng;Wan, Xiaobing [Tetrahedron,2014,vol. 70,# 51,p. 9615 - 9620]

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