Methanol → HCID 22591851, Verbindung

HRID 749512Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 749512
[NH2:1][CH:2]([C:7]1[CH:16]=[CH:15][C:10]2[O:11][CH2:12][CH2:13][O:14][C:9]=2[CH:8]=1)[CH2:3][C:4]([OH:6])=[O:5].S(Cl)(Cl)=O.[CH3:21]O>>[NH2:1][CH:2]([C:7]1[CH:16]=[CH:15][C:10]2[O:11][CH2:12][CH2:13][O:14][C:9]=2[CH:8]=1)[CH2:3][C:4]([O:6][CH3:21])=[O:5]

Komponenten

4

Edukt 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 35364503-amino-3-(2,3-dihydro-1,4-benzodioxin-6-yl)propanoic acid

Produkt 1

HCID 22591851HCID 22591851, Verbindung

Versuchsvorschrift

3-Amino-3-(2,3-dihydro-1,4-benzodioxin-6-yl)propionic acid [synthesis according to instructions known from the literature (e.g., L. Lázár, T. Martinek, G. Bernáth, F. Fülöp, Synth. Comm. 1998, 28, 219-224)]is introduced into a vessel in methanol (about 0.5 to 1.0 mol/l) and admixed dropwise at 0° C. with 1.2 eq of thionyl chloride. When the addition has been made the reaction mixture is stirred at room temperature overnight and subsequently concentrated. The residue is dissolved in a little methanol and the product is precipitated with diethyl ether. The solid is filtered off with suction, washed repeatedly with diethyl ether and dried under reduced pressure.

Aufarbeitung

  1. additionWhen the addition
  2. concentrationsubsequently concentrated
  3. dissolutionThe residue is dissolved in a little methanol
  4. customthe product is precipitated with diethyl ether
  5. filtrationThe solid is filtered off with suction
  6. washwashed repeatedly with diethyl ether
  7. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-574582ea62f643f28a2b4325e5801890
Quelldatensatz
uspto-grants-2008_07
Patentnummer
US07402683B2

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