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A kind of synthetic method of loteprednol intermediate

A technology of loteprednol etabon and intermediates, which is applied in the field of preparation of loteprednol etabon, can solve the problem of high cost of raw materials, and achieve the effects of good purity, high yield and stable process

Active Publication Date: 2022-06-14
TIANJIN PHARMA GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthetic method has the disadvantage of high cost of raw materials

Method used

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  • A kind of synthetic method of loteprednol intermediate
  • A kind of synthetic method of loteprednol intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1: Synthesis of Compound II

Embodiment 1-1

[0038] Under the protection of nitrogen, 15g 11α hydroxy-ADD (Compound I), 100ml of dichloromethane, 2ml of acetic anhydride were added to the reaction bottle, the control temperature was dropped into 10ml of phosphoric acid at 0 ~ 5 ° C, after 5 hours of insulation stirring, diluted to 10% sodium bicarbonate aqueous solution neutralized, stirred for 30 minutes, filtered, dried to give 13.6g yellow solid, molar yield 96.5%, HPLC purity 93%.

Embodiment 1-2

[0040] Under the protection of nitrogen, 100ml of tetrahydrofuran, 5g of phosphorus pentoxide was added to the reaction bottle, 15g of 11α hydroxy-ADD (Compound I) was added at a controlled temperature of 0 to 5 °C, after 5 hours of insulation and agitation, diluted to 10% aqueous sodium bicarbonate solution for neutralization, stirred for 30 minutes, filtered, dried to give 13.1g of compound II, molar yield of 92.9%, HPLC purity of 95%.

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Abstract

The present invention provides a method for preparing an ecaroteprednol intermediate. The present invention uses cheap and easy-to-obtain 11α-hydroxy-ADD as a starting material, and undergoes dehydration, Grignard, hydrolysis, oxidation, bromohydrin and reduction to obtain 17β Carboxylic acid (Compound VII). The starting material of the invention is easy to obtain, the yield is high, the purity is good, and the process is stable.

Description

Technical field [0001] The present invention relates to a method for preparing steroidal drug intermediates, in particular to a method for preparing a carboxrotepredno intermediate. Background [0002] Loteprednol Etabonate (LE) is a steroidal drug used to treat ocular inflammation, which can be applied to the treatment of blepharitis and bulbous conjunctivitis, uveitis, inflammation of the cornea and anterior segment of the eye and other corticosteroid sensitivity, as well as for the treatment of postoperative inflammation after various eye surgeries. Clodiprinol can also be used to prepare a compound formulation with tobramycin. Citiprinol suspension eye drops were first successfully developed by Pharmos Corp in the United States, and were first approved for listing in the United States in 1997 and in China in 2011. [0003] The synthesis of the ESCROTER API uses 17β carboxylic acid as an important intermediate. At present, the synthesis method of 17β carboxylic acid reported i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J3/00
CPCC07J3/005
Inventor 李蕾李志万
Owner TIANJIN PHARMA GROUP CORP
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