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Automatic synthesis method of methylation reagent [11C] CH3Br

An automated synthesis, ch3br technology, applied in organic chemistry methods, chemical instruments and methods, isotope introduction into organic compounds, etc., can solve problems such as corrosion and weak reducibility

Inactive Publication Date: 2010-08-11
THE FIRST AFFILIATED HOSPITAL OF SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since HBr is less corrosive and reductive than HI, [ 11 C]CH 3 Br is more favorable as a methylating reagent, but there is no wet automated synthesis [ 11 C]CH 3 Br and its further direct use in the methylation reaction to prepare 11 Research report on C-labeled positron drugs

Method used

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  • Automatic synthesis method of methylation reagent [11C] CH3Br
  • Automatic synthesis method of methylation reagent [11C] CH3Br
  • Automatic synthesis method of methylation reagent [11C] CH3Br

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1 11 CH 3 Br automated synthesis process

[0040] 11 CH 3 The automated synthesis process flow of Br is shown in figure 1 .

[0041] 11 CH 3 Preparations before Br synthesis. a) open 11 C-CH 3 I synthesis software control interface. b) Turn on the gas source switch of nitrogen and compressed air, and adjust the nitrogen valve to make the air pressure greater than 0.1MPa. c) regulation 11 C-CH 3 Nitrogen pressure gauge on the I module: 0.04~0.08MPa. d) Turn on accelerator production 11 CO 2 . e) Take a set of clean methyl iodide reaction tubes and large and small sealing caps, cover the sealing caps (double layers), fill the reaction tubes with nitrogen, install them into the module, cover the metal fixing cards firmly, and rivet the screws. f) Take two long needles and one short needle and insert them into the reaction tube from the double layer of the sealing cover, where the 11 CO 2 Do not insert the long needle of the reaction tube to the b...

Embodiment 2

[0044] Example 2 [ 11 CH 3 ]Triflate (with O- 11 CH 3 key) automated synthesis

[0045] [ 11 CH 3 ] Triflate automated synthesis process is shown in figure 2 . on the three-way valve 11 CH 3 A small column containing NaOH solid particles and a column containing P 2 o 5 After the powder column, then access " 11 CH 3 Br entry", put "[ 11 CH 3 ]Triflate exit" to access the collection device or access the next reaction. Turn on the computer 11 CH 3 I synthesis control interface, click the "Triflate graphic" in the lower right corner, and the air valve will be opened synchronously at this time, N 2 enter, K 8 Turn on, the furnace starts to preheat the CF 3 SO 3 Ag conversion column (a certain proportion of CF 3 SO 3 Ag and graphite powder are processed by a specific process) to 180-200°C (References 7, 8). Click "Iodomethane" → "Installation Start" → "OK" → "Start", the liquid nitrogen will drop automatically, 11 CO 2 Release for 2 minutes, and the synthesi...

Embodiment 3

[0047] Embodiment 3 (S-[ 11 CH 3 ])-L-Methionine (with S- 11 CH 3 key) and (S-[ 11 CH 3 ])-L-cysteine ​​(with S- 11 CH 3 key) automated synthesis

[0048] (S-[ 11 CH 3 ])-L-methionine (MET) and (S-[ 11 CH 3 ])-L-cysteine ​​(CYS) (ref. 9) can be obtained by 11 CH 3 Alkylation reaction of Br with the precursor L-homocysteine ​​thiolactone hydrochloride or L-cysteine ​​alkaline ethanol solution in the Sep-Pak C18 column, and through the Sep-Pak C18 column Separation and purification are obtained, and its automated synthesis process flow is in image 3 .

[0049] Preparations for the synthesis of MET and CYS. In the two-position six-way valve 11 CH 3 Add a self-made P containing P at the entry end of Br 2 o 5 powder column. In a 10 mL sterile vacuum bottle, add 0.05 M NaH 2 PO 4 Solution (pH 3 ~ 4) 5 ~ 8mL, installed into the module, and inserted into the gas and liquid pipes. A Sep-Pak C18 column activated by 5mL of ethanol and treated by 5mL of water, a st...

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Abstract

The invention relates to an automatic synthesis method of [11C] CH3Br and an automatic synthesis system thereof. The mixed gas of 0.5% O2 and 99.5% N2 is used as a target gas to produce 11CO2 by a circular accelerator through 14N (p, a) 11C nuclear reaction. 11CO2 can generate 11CH3Br by LiAlH4 reduction, hydrolysis and brominating reaction. A PET-CS-II-IT-IllCH3I synthesis module or a similar synthesis module is adopted for synthesis. [11C] CH3Br is further transformed to [11CH3] Triflate in a heated CF3SO3Ag / graphite column, and can be further used in methylation reaction to prepare [11C] methyl-N-2beta-methyl ester-3beta-(4- fluorine- phenyl) tropane. [11C] CH3Br can be used in methylation reaction to prepare 11C labeled positron medicine containing N-11CH3, O-11CH3 and S-11CH3 bonds, such as S-[11CH3]-L-methionine, (S-[11CH3])-L-cysteine and (N-[11CH3]) sinkaline and [11C] methyl-N-2beta- methyl ester-3beta-(4-fluorine- phenyl) tropane. The invention can realize the automatic synthesis of 11 CH3Br, can realize automatic synthesis, short synthesis time, high radiochemical yield and high purity quotient of radiochemical products, and can realize the automated production of 11C labeled positron medicine by further using methylation reaction.

Description

【Technical field】 [0001] The present invention relates to the application field of PET (Positron Emission Tomography positron emission tomography imaging), be specifically related to novel methylation reagent [ 11 C]CH 3 Br (ie 11 CH 3 Br) automated synthesis method, synthesis system, and its N- 11 CH 3 , O- 11 CH 3 and S- 11 CH 3 Further applications in bond methylation reactions. 【Background technique】 [0002] Positron emission tomography (PET) technology has been widely used in clinical diagnosis and treatment monitoring. PET uses the principle of photon collimation and gamma scintillation detection technology to detect the photons of annihilation radiation produced by the tracer in vitro, and the collected information is processed by a computer to display the tomographic image of the target organ and give quantitative physiological parameters. At present, PET has become a very important diagnostic tool in clinical work, especially in the early diagnosis of can...

Claims

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Application Information

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IPC IPC(8): C07C19/075C07C17/16C07C309/66C07C303/26C07B59/00C07C323/58C07C215/40C07D451/02
Inventor 唐刚华
Owner THE FIRST AFFILIATED HOSPITAL OF SUN YAT SEN UNIV
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