Acetic Anhydride → 5-Amino-3-acetoxymethyl-2,4,6-triiodobenzoic acid

HRID 1604170Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1604170
[NH2:1][C:2]1[C:3]([I:15])=[C:4]([CH2:13][OH:14])[C:5]([I:12])=[C:6]([C:10]=1[I:11])[C:7]([OH:9])=[O:8].[C:16](OC(=O)C)(=[O:18])[CH3:17]>N1C=CC=CC=1>[NH2:1][C:2]1[C:3]([I:15])=[C:4]([CH2:13][O:14][C:16](=[O:18])[CH3:17])[C:5]([I:12])=[C:6]([C:10]=1[I:11])[C:7]([OH:9])=[O:8]

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 184291945-Amino-3-hydroxymethyl-2,4,6-triiodobenzoic acid

Produkt 1

HCID 184293275-Amino-3-acetoxymethyl-2,4,6-triiodobenzoic acidAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

5-Amino-3-hydroxymethyl-2,4,6-triiodobenzoic acid (41.2 g, 0.076 mol) was dissolved in pyridine (100 ml), and acetic anhydride (80 ml) was added slowly with efficient stirring at room temperature. Stirring was continued overnight. The reaction mixture was then evaporated to a semisolid mass and treated with hydrochloric acid (2M, 250 ml). The white to grey precipitate formed was filtered off and washed with water (2×40 ml) and then dried. 44.2 g (100%) of product was isolated.

Aufarbeitung

  1. stirringStirring
  2. customThe reaction mixture was then evaporated to a semisolid mass
  3. additiontreated with hydrochloric acid (2M, 250 ml)
  4. customThe white to grey precipitate formed
  5. filtrationwas filtered off
  6. washwashed with water (2×40 ml)
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7eebdd001f054e0e90d36227527cd14e
Quelldatensatz
uspto-grants-1999_11
Patentnummer
US05993780

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