반응 #491712

반응 방정식

ether

methanesulphonic acid

aminoguanidine bicarbonate

→

Aminoguanidine Bismesylate

용매

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONWhen the addition
2. 2
   기타had fallen to ˜40°
3. 3
   workup.ADDITIONDuring the addition, colourless needles
4. 4
   여과filtered
5. 5
   세척the product washed with cold ether
6. 6
   기타dried overnight in vacuo at 50°
7. 7
   기타Yield=528 g (99.25%), mpt=149-150° (Lit: WO/2004/026845; 147.5°)

실험 절차

To a stirred solution of 99.5% methanesulphonic acid [Aldrich] (422 g; 4.40 mol) in methanol (720 cm3) at 40° was added portionwise over 30 minutes aminoguanidine bicarbonate [Aldrich] (272.0 g; 2.00 mol). When the addition was complete, the solution was stirred until the temperature had fallen to ˜40° and then treated slowly with cold ether (500 cm3). During the addition, colourless needles started to deposit. The resulting slurry was stood at 0° for 4 hrs, filtered and the product washed with cold ether and dried overnight in vacuo at 50°. Yield=528 g (99.25%), mpt=149-150° (Lit: WO/2004/026845; 147.5°)

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