Ammonium Chloride → (7-Chloro-1,3-dioxaindan-5-yl)methanol

HRID 468275

Reaktionsgleichung

Reaktionsgleichung von HRID 468275
[Cl:1][C:2]1[C:7]2[O:8][CH2:9][O:10][C:6]=2[CH:5]=[C:4]([CH:11]=[O:12])[CH:3]=1.[BH4-].[Na+].[NH4+].[Cl-]>C1COCC1>[Cl:1][C:2]1[C:7]2[O:8][CH2:9][O:10][C:6]=2[CH:5]=[C:4]([CH2:11][OH:12])[CH:3]=1

Komponenten

5

Versuchsvorschrift

To a solution of 7-chlorobenzo[d][1,3]dioxole-5-carbaldehyde (6.0 g, 33 mmol) in THF (50 mL) was added NaBH4 (2.5 g, 64 mmol)) in portions at 0° C., The mixture was stirred at this temperature for 30 mm and then poured into aqueous NH4Cl solution. The organic layer was separated, and the aqueous phase was extracted with EtOAc (50 mL×3). The combined extracts were dried over Na2SO4 and evaporated under reduced pressure to afford (7-chlorobenzo[d][1,3]dioxol-5-yl)methanol, which was directly used in the next step.

Aufarbeitung

  1. customThe organic layer was separated
  2. extractionthe aqueous phase was extracted with EtOAc (50 mL×3)
  3. dry with materialThe combined extracts were dried over Na2SO4
  4. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-721d231310dc4dd9a0ca9c705dbd586e
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08623905B2

Verknüpfte Notizen

Wird geladen…