Preparation method of prednisone acetate or analogues thereof

A technology of prednisone acetate and analogs, which is applied in the field of preparation of steroid drug intermediates, can solve the problem of high cost of starting raw materials, and achieve the effects of stable yield, high yield and high yield

Inactive Publication Date: 2014-02-26
HUNAN NORCHEM PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation method of prednisone acetate or analogues thereof
  • Preparation method of prednisone acetate or analogues thereof
  • Preparation method of prednisone acetate or analogues thereof

Examples

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Embodiment 1

[0020] oxidation reaction

[0021] At room temperature, add 180ml of glacial acetic acid and 50ml of manganese acetate aqueous solution with a mass concentration of 50% to a clean and dry 500ml four-necked round-bottomed flask equipped with a thermometer, reflux condenser, and mechanical stirring, and add 100.0g of compound I under stirring, and the system Cool down to 0 to 10°C, and add dropwise 50ml of chromium trioxide aqueous solution with a mass concentration of 50% under temperature control at 0 to 10°C. After the dropwise addition was completed, the temperature was raised to 30-35° C. to react for 2 hours. TLC followed the reaction until no raw material remained. The system was cooled to room temperature. The reaction system was added dropwise to 2L of purified water, a large amount of solids were precipitated, and the stirring was continued for 2 hours. The system was suction-filtered, the filter cake was washed with water until neutral, and then dried at 50°C to ob...

Embodiment 2

[0031] oxidation reaction

[0032] At room temperature, under the protection of nitrogen, add 200ml of acetone and 80ml of manganese acetate solution with a mass concentration of 40% to a clean and dry 500ml four-necked round-bottomed flask equipped with a thermometer, a reflux condenser, and mechanical stirring, and add 100.0g of the compound under stirring Ⅰ. The temperature of the system is lowered to 0 to 10°C, and the temperature is controlled at 0 to 10°C, and 80ml of chromium trioxide aqueous solution with a mass concentration of 60% is added dropwise. After the dropwise addition was completed, the temperature was raised to 35-37° C. to react for 3 hours. TLC followed the reaction until no raw material remained. The system was cooled to room temperature. The reaction system was added dropwise to 3 L of purified water, a large amount of solids were precipitated, and the stirring was continued for 2.5 hours. The system was suction-filtered, the filter cake was washed w...

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Abstract

The invention relates to a preparation method of prednisone acetate or analogues thereof. Prednisone acetate or the analogues therefore can be prepared from a compound I through an oxidation reaction, a cyano substitution reaction, a siloxy protection reaction, an intramolecular nucleophilic substitution reaction and an esterification reaction. The preparation method of prednisone acetate or the analogues thereof has the advantage that the starting raw material is easy to get, and the yield is high and stable. Besides, the reaction route of the preparation method is as shown in specification, wherein R1 is Cl or Br, and R is H or a C1-C10 hydroxyl.

Description

technical field [0001] The present invention relates to the preparation method of steroid drug intermediate, in particular to a kind of preparation method of prednisone acetate or its analogue. Background technique [0002] Prednisone acetate is mainly used for various acute severe bacterial infections, severe allergic diseases, collagen diseases (lupus erythematosus, nodular periarteritis, etc.), rheumatism, rheumatoid arthritis, nephrotic syndrome, severe bronchial Asthma, acute lymphoblastic leukemia, various adrenal insufficiency, etc. More potent than hydrocortisone. [0003] my country's steroid drug and its intermediate industry has reached a certain scale, and it has become the largest exporter of hydrocortisone and prednisolone in the world. At present, the synthesis of prednisone acetate or its analogues is mainly a preparation method combining biological fermentation and chemical synthesis, which has the problems of low yield and high cost. [0004] The difficu...

Claims

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Application Information

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IPC IPC(8): C07J5/00
CPCY02P20/55
Inventor 刘喜荣
Owner HUNAN NORCHEM PHARMACEUTICAL CO LTD
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