6'-Dimethyl-4'-(N-succinimidyloxycarbonyl)phenyl-10-methyl-acridinium-9-carboxylate methosulfate (DMAE-NHS) synthesis
- Product Name:6'-Dimethyl-4'-(N-succinimidyloxycarbonyl)phenyl-10-methyl-acridinium-9-carboxylate methosulfate (DMAE-NHS)
- CAS Number:115853-74-2
- Molecular formula:C29H26N2O10S
- Molecular Weight:594.5891
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Yield: 39.4%
Reaction Conditions:
in water;toluene at 110; for 20 h;
Steps:
3 Embodiment 3: DMAE·NHS preparation of acridinium ester
The 1g (2.13 mmol) 2 ', 6' - dimethyl -4 ' - (N - succinyl imino) phenyl - acridine -9 - carboxylic acid ester by adding 20 ml in toluene without water, heated to 110 °C it is completely dissolved in toluene after cooling to room temperature, add slightly cold 11 ml dry redistilled dimethyl sulfate, under the protection of the nitrogen atmosphere, 110 °C stirring for 20 hours, then cooling the solution to room temperature, then in 4 °C continuing to stir under 1 hour; the resulting mixture filtering, solid with toluene washing two times, then the yellow solid is dissolved in 60 ml dichloromethane in, heating to boiling, the maintenance of the 2 - 3 minutes, heat filter, the obtained filtrate concentrated to 40 ml of the left and right, cooling to room temperature to obtain a yellow crystal, ethyl ether washing 3 times, vacuum drying to obtain 500 mg yellow solid, yield of 39.4%.
References:
Hunan Normal University;Yin Peng;Xie Chaolong;Xia Kaifu;Yin Guoxing;Yu Ting CN106749185, 2017, A Location in patent:Paragraph 0007
115853-72-0
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