Water → 4-Bromomethyl benzoic acid 2,2,2-trichloroethyl ester

HRID 1172278

Reaktionsgleichung

Reaktionsgleichung von HRID 1172278
[Cl:1][C:2]([Cl:6])([Cl:5])[CH2:3][OH:4].CCN(CC)CC.[Br:14][CH2:15][C:16]1[CH:24]=[CH:23][C:19]([C:20](Br)=[O:21])=[CH:18][CH:17]=1.O>C(Cl)Cl>[Cl:1][C:2]([Cl:6])([Cl:5])[CH2:3][O:4][C:20](=[O:21])[C:19]1[CH:23]=[CH:24][C:16]([CH2:15][Br:14])=[CH:17][CH:18]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 8259TrichloroethanolHCID 8471TriethylamineHCID 46406714-Bromomethyl benzoyl bromide

Produkt 1

HCID 117918784-Bromomethyl benzoic acid 2,2,2-trichloroethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A solution of 2,2,2-trichloroethanol (2.46 g, 16.5 mmol) and NEt3 (1.67 g, 16.5 mmol) in CH2Cl2 (40 ml) at 0° C. was dropwise added 4-bromomethyl benzoylbromide (4.17 g, 15.0 mmol) in CH2Cl2 (20 ml) and stirred to room temperature overnight. The reaction mixture was added H2O (20 ml) and the organic layer separated. The organic layer washed with aqueous 1 M HCl (20 ml) and H2O (20 ml). The organic layer was dried over Na2SO4, filtered and the solvent evaporated in vacuo to leave the expected product as a white solid. The product was used directly in the next step without any further purification (to be filled in).

Aufarbeitung

  1. customat 0° C.
  2. customthe organic layer separated
  3. washThe organic layer washed with aqueous 1 M HCl (20 ml) and H2O (20 ml)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-61d2cf5a3ccc4acfb442a0fe0841cccd
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07834010B2

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