3-triMethylsilyloxy-7-ketolithocholic Methyl ester synthesis
- Product Name:3-triMethylsilyloxy-7-ketolithocholic Methyl ester
- CAS Number:77341-09-4
- Molecular formula:C28H48O4Si
- Molecular Weight:476.76
75-77-4
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10538-59-7
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77341-09-4
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Yield:77341-09-4 63 g
Reaction Conditions:
with triethylamine in dichloromethane at 0; for 1.33333 h;
Steps:
1
AB-3 - AB-4 was prepared as follows: 0 ° C, Trimethylchlorosilane (63.2 g) was slowly added dropwise to a solution of AB-3 (78.8 g) Triethylamine (98.7 g, 54.4 mmo 1) in dichloromethane (750 mL). 20 minutes drop finished, Stir for 1 hour. After completion of the TLC monitoring reaction, the reaction solution was stirred with water (700 mL) for 10 minutes, and the separated organic phases were dried with saturated sodium chloride and anhydrous magnesium sulfate (40 g) for about half an hour. After the residue was evaporated to dryness on a rotary evaporator, 92 g of the resulting residue was heated to 50 ° C by adding n-hexane (280 mL) to dissolve the insoluble material. The filtrate was slowly cooled to -25 ° C and stirred for 60 minutes. The solid was precipitated and filtered. The filter cake was dried under reduced pressure to give 63 g of a white solid (94% purity)
References:
CN106892954,2017,A Location in patent:Paragraph 0077; 0080; 0081
10416-59-8
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10538-59-7
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77341-09-4
15 suppliers
$452.00/250mg
4651-67-6
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77341-09-4
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474-25-9
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77341-09-4
15 suppliers
$452.00/250mg