ChemicalBook CAS DataBase List Esacure KIP 160

Esacure KIP 160 synthesis

6synthesis methods

Product Name:Esacure KIP 160
CAS Number:71868-15-0
Molecular formula:C20H22O5
Molecular Weight:342.39

N - bromo succimide (NBS)(catalyst), 1, 1' - (methanodi - 4, 1 - phenylene) double-[2 - methyl -1 - acetone] (oxidizing agent), and dimethyl sulfoxide (DMSO) were added at 100 °C stirring for 24 hours. After the reaction by adding ethyl acetate, salt water, and ethyl acetate, it combined the organic phase column chromatography separation to obtain Difunctional alpha hydroxy ketone. Yield 90%.

1,1'-(4,4'-oxydi(4,1-phenylene))bis(2-bromo-2-methylpropan-1-one)

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Yield: 90%

Reaction Conditions:

Stage #1:bis<4-(2-bromisobutyryl)phenyl> ether with sodium disulfite in water at 85; for 0.166667 h;
Stage #2: with sodium hydroxide in water;isopropyl alcohol for 0.25 h;Product distribution / selectivity;Reflux;

Steps:

3.c
The suspension of the di-bromo intermediate obtained according to Method F or G was stirred with 3g of a Na2S2θs 10% water solution at 85°Cfor 10', then diluted with 10.6g of i-propyl alcohol and 2.6g of water. To the so obtained solution 2.3g of NaOH 50% were added and after 15' at reflux the reaction was complete (TLC SiC>2, toluene/methanol 85/15). After cooling and dilution with 13.3g of water the pH was adjusted at 3 with cone. HCI. The reaction product separate as a white solid, 3g were collected by filtration (90%), mp 97°-99°C. Hl NMR(300MHz, CDCb): δ: 8.10 (d,4H); 7.07 (d,4H); 3.9 (s,2H);1 .63 (s,12H).

References:

LAMBERTI SPA WO2009/135895, 2009, A1 Location in patent:Page/Page column 16-17