2,5(10)-ESTRADIEN-3-OL-17-ONE 3-METHYL ETHER synthesis
- Product Name:2,5(10)-ESTRADIEN-3-OL-17-ONE 3-METHYL ETHER
- CAS Number:17976-32-8
- Molecular formula:C19H26O2
- Molecular Weight:286.41
1091-93-6
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17976-32-8
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$165.00/250mg
Yield: 87%
Reaction Conditions:
Stage #1:3-methoxy-17-hydroxyestra-2,5(10)-diene with 2,6-di-tert-butyl-4-methyl-phenol;cyclohexanone;aluminum isopropoxide in toluene at 108 - 110; for 1 h;
Stage #2: with water in toluene at 20 - 25; for 1 h;
Steps:
1
To a stirred solution of 106.3 g (0.52 mmol) of aluminum isopropoxide in 2000 ml of dry toluene 720 ml of cyclohexanone, 0.35 g of 2,6-ditert-butyl-4-methyl-phenol and 100 g (0.307 mol) 3-methoxy-17-hydroxy-estra-2,5(10)-diene were added, then the reaction mixture was stirred at 108-110 0C for 1 h. The reaction was followed by TLC. After completion of the reaction the mixture was cooled to 20-25 0C, 200 ml of water was added and the so obtained mixture was stirred for 1 h. The precipitated aluminum hydroxide was filtered off and the filtrate was concentrated to a volume of 250 ml under reduced pressure. A mixture of 200 ml of methanol and 100 ml of water was added to this concentrated warm - about 60 0C - solution, the obtained suspension was cooled to 20-25 °C and stirred for 1 h. The precipitated crystalline product was filtered off and dried below 40 0C in vacuum to yield 76.4 g (87%) of the title compound. Purity: min. 98% (HPLC) Melting point: 106-110 °C.
References:
RICHTER GEDEON VEGYéSZETI GYáR RT. WO2007/66158, 2007, A2 Location in patent:Page/Page column 8
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1000210-73-0
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17976-32-8
16 suppliers
$165.00/250mg
1000210-73-0
0 suppliers
inquiry
17976-32-8
16 suppliers
$165.00/250mg
111-87-5
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$6.00/100g
17976-32-8
16 suppliers
$165.00/250mg