Methanol → 4-(4,8,11-Tris-(2,2,2-trifluoroacetyl)-1,4,8,11-tetraazacyclotetradec-1-ylmethyl)-benzoic acid

HRID 507797

Reaktionsgleichung

Reaktionsgleichung von HRID 507797
[N:1]1([CH2:15][C:16]2[CH:24]=[CH:23][C:19]([C:20]([OH:22])=[O:21])=[CH:18][CH:17]=2)[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9][NH:8][CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[CH3:25][OH:26].[F:27][C:28]([F:35])([F:34])[CH2:29][O:30]C(=O)C>C(N(CC)CC)C>[F:35][C:28]([F:27])([F:34])[C:29]([N:4]1[CH2:5][CH2:6][CH2:7][N:8]([C:25](=[O:26])[C:28]([F:35])([F:34])[F:27])[CH2:9][CH2:10][N:11]([C:29](=[O:30])[C:28]([F:35])([F:34])[F:27])[CH2:12][CH2:13][CH2:14][N:1]([CH2:15][C:16]2[CH:24]=[CH:23][C:19]([C:20]([OH:22])=[O:21])=[CH:18][CH:17]=2)[CH2:2][CH2:3]1)=[O:30]

Komponenten

5

Edukt 3

HCID 887MethanolHCID 1305774-((1,4,8,11-Tetraazacyclotetradec-1-yl)methyl)benzoic acidHCID 1362562,2,2-Trifluoroethyl Acetate

Produkt 1

HCID 866162154-(4,8,11-Tris-(2,2,2-trifluoroacetyl)-1,4,8,11-tetraazacyclotetradec-1-ylmethyl)-benzoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

To a two-neck round bottom flask purged with argon was added successively 4-(1,4,8,11-tetraazacyclotetradec-1-ylmethyl)-benzoic acid (90 mg, 0.24 mmol), dry methanol (1 ml), dry triethyl amine (0.5 ml) and trifluoroethylacetate (1.7 ml). All following procedures were carried on in argon atmosphere. The mixture was stirred for 60 hours. After that the solvents were removed at reduced pressure and the residue was taken up in dry tetrahydrofurane (5 ml). The THF solution was filtered and the solvent removed at reduced pressure. The residue was dried in vacuo for 4 hours to produce 0.54 g of oily compound. MS m/z 623.5 M[C24H27F9N4O5]+1.

Aufarbeitung

  1. customTo a two-neck round bottom flask purged with argon
  2. customAfter that the solvents were removed at reduced pressure
  3. filtrationThe THF solution was filtered
  4. customthe solvent removed at reduced pressure
  5. customThe residue was dried in vacuo for 4 hours

Quellen und Nachweise

ORD-Eintrag
ord-7e80c693879d4ac3860835df41c536e3
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786292B2

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