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ChemicalBook CAS DataBase List 5,5-DIMETHYL-1-PYRROLINE N-OXIDE
3317-61-1

5,5-DIMETHYL-1-PYRROLINE N-OXIDE synthesis

3synthesis methods
To a three-necked round bottom flask equipped with a condenser, addi­tion funnel, thermometer, and mechanical stirrer and containing 300 ml. 95% ethanol precooled to 2°C is added, all at once, 14.5 g (0.1 mole) 4-methyl-4-nitropentanol, and 13.1 g (1.2 mole) zinc dust. With rapid agita­tion, the glacial acetic acid (24.0 g, 0.4 mole) is added dropwise over a 1-hr period while maintaining the reaction temperature below 15°C. The mix­ture is stirred vigorously for 2 hr and then stored in the refrigerator for 2 days, at approximately 1°C. Then the zinc acetate is filtered and rinsed with 100 ml of ethanol. The combined ethanol factions are rotoevapo-rated to give the crude nitrone. The crude nitrone is dissolved in a 200 ml portion of dichloromethane and the latter washed two times with saturated sodium bicarbonate solution. The organic layer is dried over sodium sul­fate and the solvent rotoevaporated, to give 10.7 (94% yield) of the crude nitrone. The product was purified by double distillation (b.p. 53°C, 0.1 Torr), to give 6.8 g (60%) of the pure nitrone as a white hygroscopic solid. The H1 NMR (400 MH CDC13, Me4Si) is 6.80 (t, 2H, methylene bound to quaternary C, J = 7.2Hg), 1.43 (s, 6H, methyl), C13NMr (100 MH2, CDC13, Me4 Si) 5=132.4 (Vinyl), 73.5 (quaternary), 34.1 (Allyl), 25.3 (methylene bound to quaternary C), 24.4 (methyls).
Preparation of 5,5-dimethyl-l-pyrroline-N-oxide
-

Yield:-

Steps:

Multi-step reaction with 2 steps
1.1: toluene-4-sulfonic acid
2.1: ammonium chloride; zinc / tetrahydrofuran; water / 2 h / 3 - 10 °C
2.2: 2 h / 70 °C

References:

Khoroshunova, Yulia V.;Morozov, Denis A.;Taratayko, Andrey I.;Gladkikh, Polina D.;Glazachev, Yuri I.;Kirilyuk, Igor A. [Beilstein Journal of Organic Chemistry,2019,vol. 15,p. 2036 - 2042]

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