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Preparation method of dibenzyl phosphate and tetrabenzyl pyrophosphate

A technology of tetrabenzyl pyrophosphate and dibenzyl phosphate is applied in the field of preparation of pharmaceutical intermediates and achieves the effects of low cost, mild reaction conditions and high yield

Pending Publication Date: 2022-04-22
VIWIT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This just means, utilizes this improved method and its operational route to prepare dibenzyl phosphate will be limited by carbon tetrachloride, there is certain limitation

Method used

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  • Preparation method of dibenzyl phosphate and tetrabenzyl pyrophosphate
  • Preparation method of dibenzyl phosphate and tetrabenzyl pyrophosphate
  • Preparation method of dibenzyl phosphate and tetrabenzyl pyrophosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0064] 1. Preparation of dibenzyl phosphate

[0065]

[0066] Include the following steps:

[0067] ①. Add 41kg (about 379mol) of benzyl alcohol, 41kg (about 405mol) of triethylamine and 27.0kg (about 197mol) of phosphorus trichloride to 300kg of dichloromethane. After the addition is complete, keep the temperature at 20-25°C for 30 minutes. After TLC (thin layer chromatography) detects that reaction is substantially complete (remaining amount of benzyl alcohol≤2wt%), obtain the reaction solution containing dibenzyl phosphite, cool to-3~3 ℃, add 150kg purified water to quench the reaction, stir 10min, stand still, separate the liquids, take the organic phase, extract the upper aqueous phase with dichloromethane (30kg×3) for 3 times, combine the organic phases, and then distill under reduced pressure (vacuum degree≤-0.09MPa, temperature 30~35°C) To substantially not going out distillate, obtain dibenzyl phosphite;

[0068] Further purification:

[0069] The above-mentione...

Embodiment 2

[0083]The same content as in Example 1 will not be repeated, but the difference is that in the step 1 of preparing dibenzyl phosphate, the consumption of triethylamine is adjusted to 38.5kg (about 380mol), that is: the mole of benzyl alcohol and triethylamine The ratio was 1:1, and dibenzyl phosphate was prepared as a white powdery solid with a HPLC purity of 99.1% and a total yield of 68.8% (based on benzyl alcohol).

Embodiment 3

[0085] The same content as in Example 1 will not be repeated, but the difference is that in the step 1 of preparing dibenzyl phosphate, the amount of phosphorus trichloride is adjusted to 26.1kg (about 190mol), that is: benzyl alcohol and phosphorus trichloride The molar ratio of dibenzyl phosphate was 1:0.5 to prepare dibenzyl phosphate, a white powdery solid, with a HPLC purity of 99.4% and a total yield of 72.5% (calculated as benzyl alcohol).

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Abstract

The invention discloses a preparation method of dibenzyl phosphate and tetrabenzyl pyrophosphate, and the preparation method of the dibenzyl phosphate comprises the following steps: carrying out hydroxylation reaction on dibenzyl phosphate and permanganate in an alkaline solution to generate the dibenzyl phosphate. According to the preparation method of dibenzyl phosphate, potassium permanganate and the alkaline solution are synergistically matched, so that the problem of relatively low product yield caused by excessive side reactions can be effectively avoided while dibenzyl phosphate is generated through reaction of dibenzyl phosphate; therefore, the high yield of the dibenzyl phosphate is 60% or above.

Description

technical field [0001] The invention belongs to the field of preparation of pharmaceutical intermediates, in particular to a preparation method of dibenzyl phosphate and tetrabenzyl pyrophosphate. Background technique [0002] Tetrabenzyl pyrophosphate, English name: Tetrabenzyl pyrophosphate, CAS number: 990-91-0, is an important pharmaceutical intermediate, which is used for raw materials such as fosaprepitant (the prodrug of aprepitant oral preparation) The preparation plays a pivotal role. [0003] At present, one of the main methods for preparing tetrabenzyl pyrophosphate is to condense two molecules of dibenzyl phosphate by removing one molecule of water (refer to the method disclosed in Example 6 of CN 102675369 A). This shows that the key to preparing tetrabenzyl pyrophosphate is dibenzyl phosphate. [0004] Dibenzyl phosphate can be prepared by known methods, one of which is as follows: (1) benzyl alcohol, phosphorus trichloride, and triethylamine react in toluene...

Claims

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Application Information

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IPC IPC(8): C07F9/09
CPCC07F9/094C07F9/098
Inventor 魏彦君刘希望王文才徐青景邢艳平吕霄玲
Owner VIWIT PHARMA
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