17aª‡-D-high valent alkyneestradiol-3-ethyl ester and its synthesis and preparation method, pharmaceutical composition using the said compound as active ingredient
A technology of homoethinyl estradiol and compounds, applied in medicine, the synthesis and preparation of chemically synthesized drug monomer components, the field of synthesis and preparation of 17aα-D-homoethinyl estradiol-3-ethyl ester, which can solve the problem of synthesis long steps etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0174] (1) Synthesis of estrone-3-ethyl ester (I):
[0175] Stir 100g of estrone, 66ml of pyridine, and 66ml of acetic anhydride at a constant temperature of 25°C for 6 hours, add a drying tube, slowly pour it into 600ml of water, and precipitate a white solid, leave it for 2 hours, filter it with suction, wash with a large amount of hot water until there is no pyridine smell, and dry it at 60 Dry at °C, weight 110.0g, mp: 119-121 °C, monitored by thin layer chromatography as a single component. Yield 94.8%.
[0176] (2) Synthesis of 17-cyanoestradiol-3-ethyl ester (II):
[0177] Stir 110.0g (0.352mole) estrone-3-acetate, 220g KCN, 1830ml 95% ethanol, and 950ml glacial acetic acid at a constant temperature of 25°C for 24hrs, then at a constant temperature of 75°C for 1hr, remove and let cool, and pour into 6000ml of water , precipitated a white precipitate, suction filtered, rinsed with water, drained, dried at 60°C, and weighed 110.5g. TLC shows two components, the reactio...
Embodiment 2
[0186] (1) Synthesis of estrone-3-ethyl ester (I):
[0187] Stir 100g (0.37mole) of estrone, 66ml of pyridine, and 66ml of acetic anhydride at a constant temperature of 25°C for 6hrs, add a drying tube, slowly pour into 600ml of water, a white solid precipitates, leave it for 2hrs, filter with suction, wash with a large amount of hot water until no pyridine is removed smell, dried at 60°C, weight 112.0g, mp: 119-121°C, yield 96.5%.
[0188] (2) Preparation of diazomethane:
[0189] Add 60ml of 50% NaOH solution and 200ml of ether in a 500ml flask, cool the phenol to 5°C, add 20.6g (0.2mole) of nitrosomethylurea, and add a stirring bar to gently stir the reaction for 4 hours, The ether layer was pale yellow, and the ether layer was removed with a separatory funnel, and directly proceeded to the next reaction.
[0190] (3) Synthesis of D-homoestrolone-3-ethyl ester (III):
[0191] Add 62.4g (0.20mole) into a 1000ml flask, add 300ml of ethanol and stir to dissolve, cool down t...
Embodiment 3
[0198] Take 50.0g of 17aα-D-homoethinyl estradiol-3-ethyl ester, 50.0g of medicinal starch, appropriate amount of 50% ethanol, granulate, granulate, dry, and put into 2# capsules, each containing 17aα-D- Homoethinyl estradiol-3-ethyl ester 0.1g.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More