Diethyl Ether → HCID 178505340, Verbindung

HRID 1467358Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1467358
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].C(=O)(O)O.[NH2:10][NH:11][C:12]([NH2:14])=[NH:13].CCOCC>CO>[S:2]([OH:5])(=[O:4])(=[O:3])[CH3:1].[S:2]([OH:5])(=[O:4])(=[O:3])[CH3:1].[NH2:10][NH:11][C:12]([NH2:14])=[NH:13]

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 6395Methanesulfonic AcidHCID 178513185HCID 178513185, Verbindung

Produkt 1

HCID 178505340HCID 178505340, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

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°)

Aufarbeitung

  1. additionWhen the addition
  2. customhad fallen to ˜40°
  3. additionDuring the addition, colourless needles
  4. filtrationfiltered
  5. washthe product washed with cold ether
  6. customdried overnight in vacuo at 50°
  7. customYield=528 g (99.25%), mpt=149-150° (Lit: WO/2004/026845; 147.5°)

Quellen und Nachweise

ORD-Eintrag
ord-786fd66776d9409a88be7450b5c8cc29
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09000155B2

Notizen zur Reaktion

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