ChemicalBook CAS DataBase List ETIOCHOLANOLONE ACETATE

ETIOCHOLANOLONE ACETATE synthesis

6synthesis methods

Product Name:ETIOCHOLANOLONE ACETATE
CAS Number:1482-78-6
Molecular formula:C21H32O3
Molecular Weight:332.48

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Yield:1482-78-6 100%

Reaction Conditions:

with pyridine at 0 - 25;Inert atmosphere;

Steps:

3.1

To a solution of alcohol 1 (3.0 g, 10.33 mmol) in pyridine (30 mL) at 0° C. under N₂ was added acetic anhydride (4.22 g, 41.32 mmol) dropwise, then the mixture was allowed to warm to 25° C. and was stirred at 25° C. overnight. Water was added to the reaction mixture and the resultant mixture was diluted with EtOAc. The organic phase was separated, and the aqueous phase was extracted with EtOAc. The combined organic phase was washed successively with 1 N HCl, saturated sodium bicarbonate, water, and brine. The organic phase was dried (Na₂SO₄) and evaporated to isolate the desired acetate 2 as a white solid (3.45 g, quant.). ¹H NMR (300 MHz, CDCl₃) δ 0.84 (s, 3H), 0.95 (s, 3H), 1.0-1.58 (m, 13H), 1.60-1.74 (m, 2H), 1.78-1.98 (m, 5H), 2.0 (s, 3H), 2.10 (m, 1H), 2.45 (m, 1H), 4.71 (m, 1H).

References:

US2012/282331,2012,A1 Location in patent:Page/Page column 28; 29