Triethylamine → 4-(4-Morpholinylcarbonyl)phenyl trifluoromethanesulphonate

HRID 2179576Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2179576
[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].[N:16]1([C:22]([C:24]2[CH:29]=[CH:28][C:27](O)=[CH:26][CH:25]=2)=[O:23])[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1.C(N(CC)CC)C>ClCCl>[F:1][C:2]([F:15])([F:14])[S:3]([O:6][C:27]1[CH:26]=[CH:25][C:24]([C:22]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[O:23])=[CH:29][CH:28]=1)(=[O:5])=[O:4]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 67749Trifluoromethanesulfonic anhydrideHCID 7586556(4-Hydroxyphenyl)(morpholino)methanone

Produkt 1

HCID 179828654-(4-Morpholinylcarbonyl)phenyl trifluoromethanesulphonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
-10 °C

Versuchsvorschrift

1.23 ml (7.24 mmol) of trifluoromethanesulphonic anhydride are slowly added dropwise to a solution, cooled to −10° C., of 1.0 g (4.83 mmol) of 4-(4-morpholinyl-carbonyl)phenol and 2.02 ml (14.48 mmol) of triethylamine in 20 ml of dichloromethane. The mixture is stirred at −10° C. for 30 min and then at 0° C. for 30 min. It is washed successively with 10% strength sodium bicarbonate solution, water and saturated sodium chloride solution, dried over sodium sulphate and concentrated in vacuo, and the residue is dried under high vacuum. 1.71 g (94.6% of theory) of the title compound are obtained.

Aufarbeitung

  1. waitat 0° C. for 30 min
  2. washIt is washed successively with 10% strength sodium bicarbonate solution, water and saturated sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated in vacuo
  5. customthe residue is dried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-66153291ff8e40ba9b726c9882f793e3
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09067931B2

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