Water → HCID 84045984, Verbindung

HRID 625697

Reaktionsgleichung

Reaktionsgleichung von HRID 625697
[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[CH:4][C:3]=1[CH2:10][CH2:11][C:12]([O:14]C)=[O:13].O>[OH-].[Na+].CC(O)C>[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[CH:4][C:3]=1[CH2:10][CH2:11][C:12]([OH:14])=[O:13]

Komponenten

5

Versuchsvorschrift

Methyl 3-(2-bromo-3,5-difluorophenyl)propanoate (prepared as described in Step 1, 4.3 g) in aqueous NaOH (4 M, 13.5 mL) and 2-propanol (30 mL) is heated at 50° C. for 2 hours. Water is added, the mixture washed with diethyl ether, acidified to ca. pH 5 by adding concentrated aqueous HCl, and extracted twice with diethyl ether. The combined extracts of the acidified mixture are washed with brine and volatiles evaporated under reduced pressure. The resulting material (Yield 3.6 g) is used in the next step without further purification. LC (METHOD 7): tR=0.99 min.

Aufarbeitung

  1. washthe mixture washed with diethyl ether
  2. additionby adding concentrated aqueous HCl
  3. extractionextracted twice with diethyl ether
  4. washThe combined extracts of the acidified mixture are washed with brine and volatiles
  5. customevaporated under reduced pressure
  6. customThe resulting material (Yield 3.6 g) is used in the next step without further purification

Quellen und Nachweise

ORD-Eintrag
ord-c0c3a2f4b8794fad9273437e85495432
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09308194B2

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