* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
To a stirring solutionof compound 29.1(157g, 2.7 mol) in CH30H (1.6 L) at 0°Cwas added Br2 (950 g, 5.9 moL) dropwise, and the reactionwas stirred with warming tort for 15 hr. The precipitate was collected by filtration and was washed with cold methanol to yield5 compound29.2 (450 g, 60percent) as a white solid.
32%
at 0 - 25℃; for 25 h;
To a solution of acetone (12.6 ml) in methanol (150 ml), bromine (20 ml) was added dropwise over the time of 1 h. Initially the reaction was slightly exothermic so an ice bath was applied. Upon completion of addition, the ice bath was removed and the resulting deep red reaction was stirred at 25° C. for 24 h. After such time, the reaction was cooled in an ice/acetone bath and stirred for 1 h. Filtration of the precipitate and wash with cold methanol afforded 1,3-dibromo-2,2-dimethoxy-propane (14.72 g, 32percent) as a white solid: 1H NMR (300 MHz, CDCl3) δ ppm 3.30 (s, 6 H, 2.x.OCH3), 3.59 (s, 4 H, 2.x.BrCH2).
Reference：
[1] Patent: WO2014/165075, 2014, A1, . Location in patent: Page/Page column 86; 87
[2] Patent: US2008/21032, 2008, A1, . Location in patent: Page/Page column 83
[3] Chemistry - A European Journal, 2011, vol. 17, # 2, p. 468 - 480
[4] Patent: US2009/298894, 2009, A1, . Location in patent: Page/Page column 44
[5] Patent: WO2016/44770, 2016, A1, . Location in patent: Page/Page column 752
2
[ 67-56-1 ]
[ 26562-24-3 ]
[ 22094-18-4 ]
[ 77416-08-1 ]
Reference：
[1] Journal of the American Chemical Society, 1974, vol. 96, p. 4597 - 4603
3
[ 67-56-1 ]
[ 816-39-7 ]
[ 22094-18-4 ]
Reference：
[1] Chemische Berichte, 1935, vol. 68, p. 1866 Anm.4
Under a nitrogen atmosphere, a 5L three-neck flask was charged with a starting material, <strong>[1520-70-3]ethanesulfonamide</strong> (163.5 g, 1.5 mol).Anhydrous potassium carbonate (275.8g, 2.0mol) and anhydrous DMF (1L) were stirred for 30min.Then 1,3-dibromo-2,2-dimethoxypropane (SM) (259.9 g, 1.0 mol) was added,Stir for 30 min, then raise the temperature of the reaction system to 95-100 °C.20-22 hours at this temperature,Then cool to room temperature.After that, the pH was adjusted to 2 to 3 with 0.1N HCl, and the mixture was stirred well for 2-3 hours. Then, 2L of water was added to the system to precipitate a lot of off-white solid, which was filtered and dried to obtain 134.1 g of a solid. The yield was 82.3. percent.
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