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Author: Subject: Possible OTC, 'safe' methylating agents
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[*] posted on 17-2-2020 at 16:58

It is critical that the oxalic acid is anhydrous. I have done the OrgSyn prep of dimethyl oxalate. I dehydrated the oxalic acid dihydrate by gently heating a weighed amount in an evaporating dish over moderate heat on a hot plate with occasional stirring. It took about 2 hours to lose the theoretical amount of water.

In the OrgSyn prep it is important to carry out the second recrystallization as the initial crystalline product is quite acidic to congo red paper. I have only done this prep once and realized a 61% yield of pure ester.

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Corrosive Joeseph
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[*] posted on 17-2-2020 at 22:11

Synthesis of Dimethyl Carbonate from Urea and Methanol over ZnO.
Wang, M., Zhao, N., Wei, & Sun, Y. (2005).
Industrial & Engineering Chemistry Research, 44(19), 7596–7599.

Synthesis of dimethyl carbonate from urea and methanol
Polyakov et al.
DGMK Tagungsbericht 2012(3):203-209


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