Cholesterol sulfate synthesis

Yield:1256-86-6 92.4%

Reaction Conditions:

with aminosulfonic acid in N,N-dimethyl-formamide at 68; for 2 h;Temperature;Solvent;

Steps:

2; 1; 1-1; 1-2; 1-3; 1-4; 1-5; 1-6; 1-7; 1-8; 1-9; 1-10; 3-5 Example 1: Preparation of cholesterol sulfate

General procedure: _{Put cholesterol and dimethylformamide (80mL) into a three-necked flask, heat and stir,After the cholesterol is completely dissolved, add sulfamic acid and heat to the reaction temperature,The reaction was stirred vigorously for about 2h. After the reaction is complete, the temperature is lowered to 25°C and the crystallization is stirred until the crystallization is complete.Filter, add anhydrous methanol to wash the filter cake, drain to obtain the intermediate product,Calculate the molar yield and residual cholesterol. When the other conditions above are the same,Change the amount of raw materials and the reaction temperature,Observe its influence on molar yield and residual cholesterol, and the results are shown in Table 1.}

References:

CN111100178,2020,A Location in patent:Paragraph 0076-0083; 0107-0112