Hydrocortisone acetate synthesis
- Product Name:Hydrocortisone acetate
- CAS Number:50-03-3
- Molecular formula:C23H32O6
- Molecular Weight:404.5
Yield:50-03-3 99%
Reaction Conditions:
with pyridine at 0 - 25; for 24 h;
Steps:
3 Synthesis of Bl.
To a solution of Al (50 g, 14 mmol,) in py (500 mL) was added AC2O (21 g, 210 mmol) dropwise at 0°C. The reaction was stirred at 25°C for 24 hrs. The mixture was poured into 4 L of water. After stirring at 25°C for 0.5 h, the mixture was filtered. The solid was washed with HC1 (1 L, 1 M) and dried to give Bl (55 g, 99%) as a solid. 1H NMR (400 MHz, CDC13) 5 5.69 (s, 1H), 5.03 (d, J= 17.6 Hz, 1H), 4.85 (d, J = 17.6 Hz, 1H), 4.51-4.44 (brs, 1H), 2.85-2.70 (m, 1H), 2.55-2.40 (m, 2H), 2.39-2.32 (m, 1H), 2.30-1.95 (m, 9H), 1.91- 1.79 (m, 2H), 1.75-1.66 (m, 2H), 1.52-1.40 (m, 5H), 1.20-0.97 (m, 3H), 0.97 (s, 3H).
References:
WO2018/9867,2018,A1 Location in patent:Paragraph 00247
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