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ChemicalBook CAS DataBase List 3-Oxopregn-4-ene-20-carbaldehyde
24254-01-1

3-Oxopregn-4-ene-20-carbaldehyde synthesis

3synthesis methods
60966-36-1 Synthesis
21-hydroxy-20-methylpregn-4-en-3-one

60966-36-1
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Yield:24254-01-1 84.7%

Reaction Conditions:

with sodium chlorine monoxide;2,2,6,6-Tetramethyl-1-piperidinyloxy free radical;Sodium hydrogenocarbonate;sodium bromide;anhydrous sodium sulphite in methanol;water monomer at 10 - 15; under 2250.23 - 3000.3 Torr; for 0.138889 h;Solvent;Reagent/catalyst;Temperature;

Steps:

1-5 Example 2 Preparation of intermediate PGT2 crude product under microchannel reactor conditions

Weigh PGT1 (66.0g) into methanol (528.0g),Stir to dissolve, marked as solution A for use;Weigh TEMPO (3.3g),Sodium bromide (5.0g) and sodium bicarbonate (5.1g) were added to purified water (500.0g),Stir to dissolve, marked as solution B for use;Weigh 227.0g of sodium hypochlorite solution (available chlorine content is 7.0%),Marked as solution C for use;Sodium sulfite (3.3 g) and water (66.0 g) were added to the reaction solution collection bottle, and the mixture was stirred and dissolved for later use.The flow rates of the feed pumps corresponding to solution A, solution B and solution C were set to 12.8mL/min, 12.2mL/min and 9.6mL/min, respectively.The residence time was 140 seconds, the temperature of the reactor was set to 10-15°C, and the pressure of the back pressure valve was adjusted to 3-4 bar.After the temperature, pressure and flow rate are stable, start the reaction timing,After 6 minutes, the reaction solution was collected, and the reaction solution was collected into a reaction solution collection bottle under stirring.The consumption of solution A completely stops the reactor,After stirring for 30 min, concentrated to remove methanol, cooled to 20-25 for 1 h, and filtered.The filter cake was washed with 66.0 g purified water and filtered,After drying at 50°C for 12h, crude PGT2 was obtained (64.5g, yield 98.3%, purity 94.7%).

References:

CN114380879,2022,A Location in patent:Paragraph 0044-0054